Dung Quat Refinery Light Naphta Isomerization Unit

PROCESS DATA SHEET
Project N° - Unit Doc. type Equipment N° Serial N° Rev. index
8474L-023 ML 001 A
Op. Center JOB No.
Op. Center Doc. No.
DOCUMENT CLASS X FEED Doc. No.
CLIENT PETROVIETNAM Page
LOCATION DUNG QUAT PENEX UNIT (023)

VIETNAM A
OPERATING MANUAL
UNIT 023
PENEX
Rev. A Rev.
Page Page
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A 27-JUL-07 C. VERDON J-P. BINET R. LEFEBVRE ISSUE FOR REVIEW

Date
Rev. Written by Checked by Approved by Description
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Document revisions
PDS94 - Rev. 4 - ANG - XL97 H:\projet\8475M-DQR-POC\08-Process\Operating Manuals\operating manual - DQR\ISOM\[8474L-023-ML-001-A.xls]PAGE A PD094A14
VIETNAM OIL AND GAS CORPORATION
(PETROVIETNAM)
DUNG QUAT REFINERY
OPERATING MANUAL
VOLUME 13
LIGHT NAPHTA
ISOMERIZATION UNIT
UNIT 023
BOOK 1/2
Rev. 0
VIETNAM OIL AND GAS CORPORATION (PETROVIETNAM) March 2007
DUNG QUAT REFINERY Rev. :0
OPERATING MANUAL Chapter : 1
UNIT ISOM (023) Page :1/2
CONTENTS
CHAPTER 1 BASIS OF DESIGN

1. DUTY OF THE PLANT
2. ENVIRONMENTAL CONDITIONS
3. FEEDSTOCKS AND PRODUCTS SPECIFICATIONS
4. OVERALL MATERIAL BALANCE OF THE UNIT
5. BATTERY LIMIT CONDITIONS
6. DESIGN FEATURES
7. GAS AND LIQUID EFFLUENTS
CHAPTER 2 PROCESS DESCRIPTION

1. PROCESS THEORY
2. DESCRIPTION OF FLOW
CHAPTER 3 DESCRIPTION OF UNIT CONTROL

1. DESCRIPTION OF FLOW WITH CONTROLS
2. OPERATING CONDITIONS
3. PROCESS VARIABLES
4. INTER-UNIT CONTROL SCHEME
5. UNINTERRUPTIBLE POWER SUPPLY (UPS)
6. COMPLEX CONTROL DESCRIPTION
CHAPTER 4 UILITY, CHEMICAL AND CATALYST REQUIREMENTS

1. UTILITIES
2. CHEMICALS CONSUMPTION
CHAPTER 5 PREPARATION FOR INITIAL START-UP

1. PLANT CHECK-OUT
2. LINE FLUSHING
3. WATER CIRCULATION
4. LEAK TESTING
5. HEATER DRY-OUT
6. LOADING OF METHANATOR, DRIERS, SCRUBBER AND REACTORS
7. CHEMICAL CLEANING
CHAPTER 6 INITIAL AND NORMAL START-UP

1. SUMMARY OF START-UP
2. PURGING AND GAS BLANKETING
3. METHANATOR START-UP
4. HYDROCARBON CIRCULATION AND INITIAL DRYDOWN
5. ACIDIZING AND FINAL DRYDOWN
6. CATALYST LOADING
7. INITIAL START-UP
8. NORMAL START-UP
9. DEISOHEXANIZER START-UP
10. NORMAL OPERATION
CHAPTER 7 NORMAL SHUTDOWN

1. NORMAL SHUTDOWN PROCEDURES
UNIT ISOM (023) Page :2/2
2. CATALYST UNLOADING AND HANDLING PROCEDURES

3. SPECIAL PROCEDURES
CHAPTER 8 EMERGENCY SHUTDOWN PROCEDURES

1. INTRODUCTION
2. EMERGENCY FUNCTIONS PHILOSOPHY
3. PROCESS FAILURES
4. UTILITY FAILURES
5. MAJOR UPSETS
CHAPTER 9 SAFETY EQUIPMENT AND PROCEDURES

1. PRESSURE SAFETY DEVICES
2. ALARM SETTINGS
3. TRIP SETTINGS
4. TRIP SYSTEM CHART
5. CAUSE AND EFFECT DIAGRAM
6. MATERIAL HAZARD DATA SHEETS
7. SAFEGUARDING MEMORANDUM
CHAPTER 10 INSTRUMENT DATA

1. CONTROL VALVES AND INSTRUMENTS
2. ORIFICE PLATES
CHAPTER 11 SUMMARY OF MAJOR EQUIPMENT

1. EQUIPMENT LIST
2. LARGE ROTATING EQUIPMENTS
3. HEATERS
4. OTHER VENDOR INFORMATION
CHAPTER 12 ANALYSIS
1. INTRODUCTION
2. SAMPLING SCHEDULES / APPROVED TEST METHODS
3. ANALYTICAL METHODS
4. ON-LINE ANALYZERS
CHAPTER 13 PROCESS CONTROL

1. DISTRIBUTED SYSTEM CONTROL (DCS)
CHAPTER 14 DRAWINGS
1. PLOT PLAN AND HAZARDOUS CLASSIFICATION
2. PROCESS FLOW DIAGRAMS AND MATERIAL SELECTION DIAGRAMS
3. PIPING AND INSTRUENTATION DIAGRAMS
4. OTHER DRAWINGS
UNIT ISOM (023) Page : 1 / 16
CHAPTER 1
BASIS OF DESIGN
CONTENTS
1.1 LICENSOR
1.2 FUNCTION OF THE UNIT
2.1 AIR TEMPERATURE
2.2 RELATIVE HUMIDITY
2.3 RAINFALL
2.4 SNOWFALL
2.5 AIR BAROMETRIC PRESSURE
2.6 WIND
2.7 ATMOSPHERE
2.8 MISCELLANEOUS DATA
3.1 FEEDS CHARACTERISTICS

3.1.1 HYDROTREATED LIGHT NAPHTHA
3.1.2 MAKEUP GAS
3.2 PRODUCTS SPECIFICATIONS

3.2.1 ISOMERATE
3.2.2 NET GAS
4.1 PROCESS INLET

4.2 PROCESS OUTLET
5.1 FEEDSTOCKS BATTERY LIMIT CONDITIONS
5.2 PRODUCTS BATTERY LIMIT CONDITIONS
5.3 UTILITIES BATTERY LIMIT CONDITIONS
6. DESIGN FEATURES
6.1 EQUIPMENT OUTSIDE LICENSOR SCOPE
6.2 MANDATORY SUPPLY

6.2.1 SULFUR ABSORPTION AND METHANATION CATALYSTS
6.2.2 ISOMERIZATION REACTOR CATALYST
6.2.3 MOLECULAR SIEVES
6.2.4 DRCS

1.1 LICENSOR
The Penex / DIH Process (Unit 023) is based on the UOP (Universal Oil Products)
process. The Licensor has issued the following documents:
♦ UOP Project Specification (Project 928504).
♦ UOP Penex Process Hydrogen Once Through: General Operating Manual.
♦ UOP Deisohexanizer: General Operating Manual.
♦ UOP Methanator Information (Additional section of the Penex Process Hydrogen
Once Through General Operating Manual).
1.2 FUNCTION OF THE UNIT
The function of the Penex / DIH Unit is to process straight run light naphtha from the
overhead of the Naphtha Splitter column T-1202 (Unit 012) to produce a high octane
isomerate naphtha product. The light straight run naphtha is derived from either 100%
Bach Ho Crude or Mixed Crude (85% Bach Ho / 15% Arabian Light). The Penex unit is
designed for a capacity of 231 613 metric tonnes per year (equivalent to 6500 BPSD).
The UOP Penex Process is a continuous catalytic isomerization of pentanes, hexanes
and mixtures thereof, based on an equilibrium reaction. The reactions take place in a
hydrogen atmosphere, over a fixed bed of catalyst and at operating conditions, which
promote isomerization and minimize hydrocracking. This product is a mixture of iso-
paraffins with a high octane number.
The process is simple and straightforward in design and operation and trouble-free in
performance permitting a minimum of staffing and supervision. Operating conditions are
not severe as reflected by moderate operating pressure, low temperature, high catalyst
space velocity and low hydrogen partial pressure requirements.
Except for normal hydrotreating, the PENEX Process requires neither special feed
pretreatment nor especially sharp prefractionation for removal of C6 cyclics or C7+. Penex
affords the refiner considerable flexibility in the choice of feedstocks both at the time of
design or after the unit is constructed.
The major elements of the Penex / DIH Unit are the liquid feed and make-up gas driers,
the methanator, the feed surge drum, the reactors and associated heater and
exchangers, the product stabilizer, the net gas scrubber and the deisohexanizer.
Although not essential to the success of the process, the Penex system will normally
employ two reactors in a series flow configuration with the total required catalyst loading
being equally distributed between the vessels. Valving and piping are provided which
permit reversal of the processing positions of the vessels and the isolation of either for
partial catalyst replacement. With time, the Penex catalyst will become deactivated by
water, not hydrocarbon. Because the water deactivation proceeds as a sharp front,
which moves down the bed in a piston-like fashion, catalyst downstream of the front
remains unaffected. When catalyst in the lead reactor is spent, the reactor is taken off
line for reloading. During the short period of time the reactor is out of service, the second
reactor is capable of maintaining continuous operation at design throughput and yield;
conversion is moderately lower. After catalyst reloading is completed, the processing
positions of the two reactors may be reversed.
The two reactor design permits essentially 100% unit onstream efficiency and reduces
catalyst consumption costs by making partial catalyst replacements practical. It also
permits the unit to be designed for a smaller catalyst inventory (higher space velocity)
thus reducing catalyst capital requirements. Isomerization and benzene hydrogenation
reactions are both exothermic and the temperature increases across the reactor.
Equilibrium requires that the outlet temperature be as low as the activity of the catalyst
permits. With a single reactor, this would lead to a low inlet temperature and low
isomerization rates in part of the catalyst bed. The two reactor system permits the
imposition of an inverse temperature gradient by cooling between reactors through
exchange against cold feed. The first reactor may, therefore, be operated at a higher
temperature and achieve a higher reaction rate. This reduces the inventory of catalyst
and the reactor size required. Most of the isomerization is thus accomplished at high rate
in the first reactor and the final portion is performed at a lower temperature to take
advantage of the more favorable equilibrium.
Not all catalysts are suitable for application of the inverse temperature gradient principle.
Some might coke or sludge if operated at a higher inlet temperature, or else they might
promote excessive hydrocracking and yield loss. Since the Penex catalyst does neither
of these, the inverse gradient can be applied to economic advantage.
Chloride promoter (perchloroethylene) is added continuously with the feed and is
converted to hydrogen chloride in the reactor. Since the catalyst functions with very small
amounts of promoter (measured in parts per million), it is not necessary to provide
separate equipment for recovery and re-use of hydrogen chloride. It is permitted to leave
the unit by way of the stabilizer gas. The quantity of stabilizer gas is small, due to the
selective nature of the catalyst, which permits very little hydrocracking of the
pentane/hexane charge to take place.
To protect the catalyst, the liquid feed is first charged to the feed dryers and then to the
charge surge drum. Hydrogen make-up gas is sent to a methanator to remove trace
levels of CO, CO2 and H2S and then onto the make-up gas dryers prior to be mixed with
the combined feed from the charge surge drum and sent to the reactors.
The effluent from the reactor is charged to a stabilizer to remove the residual hydrogen
from the reaction and the light gases (C1 through C4) introduced with the make-up gas
and produced in the reactor as a result of cracking. The stabilizer gas is scrubbed for
hydrogen chloride removal before entering the refinery fuel gas system (Unit 037).
The catalyst itself is non-corrosive in the plant and, despite the presence of small
amounts of hydrogen chloride during operation, the dryness of the system permits
construction of carbon steel.
Bottom stream from the stabilizer is sent to the deisohexanizer (DIH) column. The DIH
primarily separates C5, 2,2-dimethylbutane and 2,3-dimethylbutane from the other C6
isomers and heavier components of the isomerate. The benefit of the addition of a DIH
column is to upgrade to a product with an octane value of 88.0 - 90.0 RONC. Compared
to a maximum research octane number of approximately 84.0 RONC for a hydrocarbon
once-through operation, this is a significant increase.
More benefits from a DIH column are derived as the C5/C6 ratio of the fresh charge
decreases since the nC5 is not recycled back to the reactor section for further
isomerization.
The DIH overhead product, composed primarily of C5's and dimethylbutanes, is sent to
storage for gasoline blending. The bottoms, flow-controlled at a small rate, are also
typically sent to storage with the DIH overhead product; however, the bottoms should be
evaluated as potential reformer feedstock as well. The bottoms draw is necessary to
avoid a build-up of heavies in the reactor section charge.
The DIH side draw, composed primarily of methylpentanes, some dimethylbutanes and
nC6, is recycled back on flow control to the isomerization unit upstream of the reactors.
Hereafter are supplied the following documents:
Diagrams showing all process and utilities connections with other units
Overall block flow diagram of the Refinery
Light naphtha from unit 012 Isomerate to TK-5106 A/B

PENEX / DIH
PROCESS
Make-up gas from unit 012 (UNIT 023) Net gas to FG (unit 037)
20°Be Caustic from unit 039
MP steam MP condensate
LP steam LP condensate
CW supply CW return
Service water PENEX / DIH Flare to unit 057

PROCESS
Cold BFW (UNIT 023)
Refinery Nitrogen Oily water
Instrument air
Plant Air
Potable water
2.1 AIR TEMPERATURE

a. Maximum recorded 41.4 °C
b. Minimum recorded 12.4 °C
c. Maximum monthly average 34.4 °C
d. Minimum monthly average 18.9 °C
e. Design maximum 36.0 °C
f. Design minimum 16.0°C
2.2 RELATIVE HUMIDITY
a. Maximum monthly average 89%
b. Minimum monthly average 80%
c. Average monthly humidity 85%
d. Design maximum 100%
e. Design minimum 40%
2.3 RAINFALL
a. Maximum recorded annual 3052 mm
b. Minimum recorded annual 1374 mm
c. Average annual 2268 mm
d. Maximum recorded in 24 hours 525 mm
e. Maximum rainfall intensity 40 mm for 10 min period
60 mm for 30 min period
108.1mm for 60 min period
2.4 SNOWFALL
Not applicable
2.5 AIR BAROMETRIC PRESSURE
a. Maximum 1023.6 mbar
b. Minimum 988.8 mbar
c. Average 1009 mbar
d. Design 1013 mbar
2.6 WIND
a. Average velocity 3.2 m/s
b. Maximum hourly velocity 42 m/s
Direction % of time for each Quadrant

No wind 43.8
N/NE 9.7/6.2
W/NW 4.1/14.3
E/SE 12.8/6.7
S/SW 1.1/1.0
The maximum velocity over a 2 minutes is 41.6 m/s for a return period of 50 years.
The maximum velocity over a 2 minutes is 32.7 m/s for a return period of 20 years
2.7 ATMOSPHERE
a. Extreme moisture - tropical climate
b. Marine exposure - salt spray
c. Sand storms - not applicable
d. Copper-attacking fumes - sulphur
e. Exposure to conductive or corrosive dusts (carbon, iron oxide, ammonium nitrates or

phosphates, etc): NO
f. Exposure to corrosive agents (nitric or sulphuric acids, chlorine, caustic, etc): NO
g. Exposure to other pollutants originating from surrounding industrial plant: YES
2.8 MISCELLANEOUS DATA
a. Frost Level Not applicable
b. Typhoon frequency 2 to 3 per year
c. Thunderstorm frequency 102 storm days per year
d. Temperature inversion occurrence Not applicable
e. Earthquakes to be taken into account and design shall be as per code UBC, zone
2
f. The site is subjected to possible flood condition
3.1 FEEDS CHARACTERISTICS
3.1.1 HYDROTREATED LIGHT NAPHTHA

The Penex / DIH unit is designed to process straight run hydrotreated light naphtha,
coming from Naphtha hydrotreating unit (Unit 012), derived from 100% Bach Ho or
Mixed crude oils (85% Bach Ho and 15% Dubai crude) at a design capacity of 6500
BPSD.
Following UOP’s evaluation of the full range naphtha for the 100% Bach Ho case and
the Mixed case, the naphtha composition has been determined to be identical for both
cases except for the higher sulfur in the Mixed case. Accordingly only a single design
case based on 100% Bach Ho with a maximum sulfur level content of 100 ppm wt shall
be used as the basis of design for the NHT/Penex-DIH and the CCR Paltformer
Complex. The NHT/Penex-DIH and the CCR Paltformer shall be capable of processing
both cases.
The feed definition for the Penex / DIH unit has the following properties:
Feed rate = 6500 BPSD.

Turndown = 3250 BPSD.
Property Value Test Method

Density at 15°C 0.674 ASTM D 4052
Composition, mole% UOP 551
N-Butane 1.16
Iso-Butane 0.12
Iso-Pentane 11.34
N-Pentane 19.00
Cyclopentane 0.12
2,2-Dimethylbutane 0.74
2,3-Dimethylbutane 1.62
2-Methylpentane 11.72
3-Methylpentane 6.34
N-Hexane 25.86
Total C5, wt. % 30.5 min.

Benzene, wt. % 6.3 max.
C7+, wt. % 3.8 max.
Total C6 Naphtenes, wt. % 11.9 max.
Methylcyclopentane 6.09
Cyclohexane 5.81
Benzene 6.30
N-Heptane 3.78
Water Saturated at design temperature UOP 481
Mol. Weight, kg/kg mole 80.48
Copper, wt. ppb 20 max. UOP 144
Lead, wt. ppb 10 max. UOP 350
Arsenic, wt. ppb 1 max. UOP 296
Fluorides Not Detectable UOP 619
Bromine Number 4.0 max. UOP 304
Chlorides, wt. ppm 0.5 max. UOP 395
Total Sulfur, wt. ppm 0.1 max. ASTM D-4045
Total Nitrogen, wt. ppm 0.1 max. ASTM D-4629
Total Oxygenates (excluding Method based on
0.5 max.
water), wt. ppm suspected compound
3.1.2 MAKEUP GAS

Make-up gas for the Penex / DIH Unit is delivered from the 3rd stage discharge of the
make-up gas multi-stage compressors C-1202A/B/C (Unit 012) at a pressure of 42.3
kg/cm2 (g). It is a product of CCR platforming unit (Unit 013).
The composition of hydrogen is the following in normal operation:
Make-up Hydrogen
Compound
mole %
H2 93.3
Methane 2.5
Ethane 2.4
Propane 1.4
i Butane 0.1
n Butane 0.1
i Pentane 0.04
n Pentane 0.02
C6+ 0.04
3.2 PRODUCTS SPECIFICATIONS
3.2.1 ISOMERATE
For the total refinery, two design cases are specified: a Design case corresponding to
6500 BPSD (Light Naphtha with cut points C5 - 82°C / high benzene feed) and an
Alternate case corresponding to 5336 BPSD (Light Naphtha with cut points C5 - 70°C /
low benzene feed). The isomerate properties depend on the operating case and on the
reactors catalyst level of activation.
Hereafter are given the composition of the isomerate obtained for each case at Start Of
Run (fresh catalyst) and End Of Run (spent catalyst).
Property Value
C5+ Product Yield at Start-of-Run, 95.2

(wt. % Fresh Feed, minimum)
C5+ RONC 87
C5+ MONC 85
RVP, kg/cm² 0.82
Benzene, vol.-% 0
Aromatics, vol.-% 0
Olefins, vol.-% 0
Sulfur, wt-ppm 1 max.
Nitrogen, wt-ppm 1 max.
Oxygenates, wt-ppm 1 max.
Design Case Alternate Case

PROPERTY
SOR EOR SOR EOR
Density at 15°C 0.656 0.656 0.647 0.648
Composition, kmol/h
Propane Trace Trace Trace Trace
Iso-Butane 0.79 0.58 0.20 0.14
N-Butane 1.67 1.35 0.73 0.61
Iso-Pentane 108.87 104.52 99.34 95.85
N-Pentane 33.69 38.76 28.49 32.65
Cyclopentane 0.33 0.35 0.33 0.35
2,2 Dimethylbutane 104.08 79.78 110.00 95.94
2,3 Dimethylbutane 18.83 22.92 10.90 14.19
2-Methyl pentane 31.44 46.70 16.26 24.65
3-Methyl pentane 5.18 9.13 2.63 4.56
N-Hexane 0.45 0.77 0.30 0.47
Methylcyclopentane 0.44 0.84 0.13 0.23
Cyclohexane 3.28 3.00 1.36 1.27
Benzene Trace Trace Trace Trace
2-Methylhexane 0.20 0.26 Trace Trace
N-Heptane 0.16 0.26 Trace Trace
Methylcyclohexane 25.39 22.24 8.21 7.74
3.2.2 NET GAS

A net gas stream will be produced from the overhead of the Stabilizer and will be routed via
a caustic scrubber for hydrogen chloride removal before being sent to Fuel Gas Unit (Unit
037).
The composition of this gas is given hereafter for the different cases:

Compound
SOR EOR SOR EOR
H2O, %mol 0.9 0.9 0.9 0.9
H2, %mol 41.6 43.3 52.9 55.0
Methane, %mol 8.0 7.9 6.8 6.7
Ethane, %mol 7.1 6.6 6.3 5.7
Propane, %mol 14.9 14.3 5.8 5.6
Iso-Butane, %mol 20.0 18.7 15.4 13.4
N-Butane, %mol 7.1 7.7 10.5 11.0
Iso-Pentane, %mol 0.4 0.6 1.3 1.7
N-Pentane, %mol 0.0 0.0 0.1 0.1
4.1 PROCESS INLET

SOR EOR SOR EOR
Hydrotreated light naphtha, kg/h 28960 28960 23242 23242
Make-up gas, kg/h 609 598 336 330
Chloride, kg/h 9 9 7 8
TOTAL 29578 29567 23585 23580
4.2 PROCESS OUTLET

SOR EOR SOR EOR
Isomerate, kg/h 27617 27724 22436 22510
Net gas, kg/h 1956 1838 1146 1063
TOTAL 29573 29562 23582 23573
The total refinery site is divided in blocks. Every block contains one or more units. The
isomerization unit is situated together with NHT and CCR units (012 and 013). Because
of this construction there are two types of battery limits: battery limits for units and battery
limits for blocks. For feedstocks and products the unit battery limit conditions for the
process streams are given. For utilities the block battery limits are given.
All the process lines entering/leaving the considered block are represented on PID
8474L-012-PID-0021-001 whereas the process lines leaving NHT/CCR or PENEX units
but not leaving the block are represented on PID 8474L-012-PID-0021-002. Utility lines
are represented on utility PIDs.
5.1 FEEDSTOCKS BATTERY LIMIT CONDITIONS

DESIGN CONDITIONS AT OPERATING CONDITIONS
ORIGIN B/L AT B/L
PRESSURE (1) TEMPERATURE PRESSURE (1) TEMPERATURE
Kg/cm2 (g) (°C) Kg/cm2 (g) (°C)
Hydrotreated Unit 012 16.0 120 7.0 38
light naphtha
Makeup gas Unit 012 48.0 160 42.3 38
5.2 PRODUCTS BATTERY LIMIT CONDITIONS

DESTINATION B/L AT B/L
PRESSURE (1) TEMPERATURE PRESSURE (1) TEMPERATURE
Kg/cm2 (g) (°C) Kg/cm2 (g) (°C)
Isomerate U051 16.0 65 3.5 37
Net gas U037 (Fuel Gas) 14.5 160 4.7 38
Note: (1) At grade – Unit 023 Battery Limit elevation is 6 m.
5.3 UTILITIES BATTERY LIMIT CONDITIONS

DESTINATION / B/L AT B/L
ORIGIN PRESSURE (1) TEMPERATURE PRESSURE (1) TEMPERATURE
Kg/cm2 (g) (°C) Kg/cm2 (g) (°C)
UTILITIES SUPPLY
MP steam OSBL 16.8 320 14.1 (3) 250
LP steam OSBL 6.3 230 3.6 (3) 160
Cold Boiler OSBL 16.3 115 4 (2) 60
Feedwater
Instrument Air OSBL 10.5 65 7.5 (2) 35
Refinery OSBL 11.7 65 7 (3) 30
Nitrogen
Cooling Water OSBL 9.2 70 5.2 (3) 32
Plant Air OSBL 10.5 65 7.5 (2) 35
Service Water OSBL 14.2 60 5 (2) 30
Potable Water OSBL 5.5 60 2.5 (2) 30
20° Be Caustic OSBL 5.5 70 1.5 (2) 40
UTILITIES RETURN
MP Condensate OSBL 16.8 320 7.5 (3) 170
LP condensate OSBL 6.3 230 2 (3) 133
Cooling Water OSBL 9.2 70 2.2 (3) 47
Oily Water OSBL 4.7 65 3.5 (3) 36
Flare OSBL 3.5 210 0.2 (1) 38
Notes: (1) At grade – Units 012/013/023 Battery Limit elevation is 15 m.

(2) At grade – Units 012/013/023 Battery Limit elevation is 12 m.
6. DESIGN FEATURES
6.1 EQUIPMENT OUTSIDE LICENSOR SCOPE
Neutralization of spent caustic

The net gas stream produced from the overhead of the stabilizer is routed to the net gas
scrubber (T-2302) for hydrogen chloride removal before being sent to Fuel Gas (Unit 037).
This is accomplished by contacting the rising acidic gases with a 10 wt% caustic solution.
The caustic is to be changed out before it falls below 2 wt%, therefore, periodically (once a
week), a portion of caustic is withdrawn to a degassing drum (D-2305) and sent by gravity to
a Neutralization Pit TK-2399. This stream contains NaClO which needs to be neutralized.
This is done with sulfuric acid on pH control, which acts as an oxygen scavenger. The
neutralized spent caustic is then routed to the oily water sewer by means of the
Neutralization Pit Eductor (J-2399).
The Neutralization Pit Eductor (J-2399) and the Neutralization Pit (TK-2399) are part of the
Isomerization Unit but are outside Licensor scope.
6.2 MANDATORY SUPPLY
6.2.1 SULFUR ABSORPTION AND METHANATION CATALYSTS

Catalyst type required for sulphur absorption in Methanator vessel (R-2301) is Puraspec
2010 from Johnson Matthey. This catalyst has a density of 1155 kg/m3 and the installed
volume is of 0.43 m3. It shall be replaced approximately every 3 years.
Catalyst type required for methanation reaction in Methanator vessel (R-2301) is
Puraspec 2443 from Johnson Matthey. This catalyst has a density of 1105 kg/m3 and the
installed volume is of 2.21 m3. It shall be replaced approximately every 3 years.
Sulfur absorption and methanation catalysts are sock-loaded into the methanator.
MSDS will be in the attachments.
6.2.2 ISOMERIZATION REACTOR CATALYST
Isomerization catalysts required are I-8 Plus and I-82 Penex Catalysts from UOP. They
are amorphous, chlorided alumina, light paraffin isomerisation catalysts containing
platinum, optimized for use in Penex units. They selectively convert normal butane,
pentane and hexane to high octane branched hydrocarbons. In addition to isomerisation
of paraffins, they also saturate benzene.
Initially lead reactor is loaded with I-8 Plus catalyst and lag reactor with I-82 catalyst.
These catalysts have a density of 885 kg/m3 and the installed volume is of 24.7 m3 per
reactor. They shall be replaced approximately every 6 years.
The I-8 Plus/I-82 Penex catalysts are dense loaded into the reactors.
MSDS will be in the attachments
6.2.3 MOLECULAR SIEVES
Molecular sieves required for Makeup Gas Driers (DR-2301/2302) shall be Molsiv
Adsorbent type PDG-418 from UOP. Sieves density is of 660 kg/m3 and the installed
volume is of 1.97 m3 per drier. Molecular sieves shall be replaced approximately every 3
years.
Molecular sieves required for Feed Driers (DR-2303/2304) shall be Molsiv Adsorbent
type HPG-250 from UOP. Sieves density is 640 kg/m3 and the installed volume is of 5.90
m3 per drier. Molecular sieves shall be replaced approximately every 3 years.
Molecular sieves are normally sock-loaded into the driers.
MSDS will be in the attachments
6.2.4 DRCS
The selected UOP Drier Regeneration Control System (DRCS) is mandatory for the
Makeup Gas Driers and the Feed Driers.
For the regeneration operation of these driers, refer to Chapter 6 (6.7. Normal operation).
Refer to attached document: “Effluent Summary Table” – 8474L-200-NM-6200-002.

UNIT ISOM (023) Page :1 / 31
CHAPTER 2
DESCRIPTION OF PROCESS
CONTENTS
1. PROCESS THEORY
1.1 PROCESS PRINCIPLES
1.2 REACTION MECHANISMS

1.2.1 FRIEDEL-CRAFTS CATALYST
1.2.2 DUAL-FUNCTION HYDRO-ISOMERIZATION CATALYST
1.3 HISTORY OF CATALYST

1.3.1 FRIEDEL-CRAFTS TYPE CATALYST
1.3.2 HYDRO-ISOMERIZATION CATALYSTS ABOVE 200°C
1.3.3 HYDRO-ISOMERIZATION CATALYSTS BELOW 200°C
1.4 OTHER REACTIONS

1.4.1 NAPHTENE RING OPENING
1.4.2 NAPHTENE ISOMERIZATION
1.4.3 BENZENE SATURATION
1.4.4 HYDROCRACKING
1.5 METHANATION
1.6 ACIDIZING
1.7 CHLORIDE PROMOTER
1.8 CAUSTIC SCRUBBING
1.9 DE-ISOHEXANIZER (DIH): THEORY OF FRACTIONATION
2.1 FEED DRIERS (DR-2303/2304) (P&ID 023-PID-0021-013)
2.2 METHANATOR (R-2301) (P&ID 023-PID-0021-010)
2.3 MAKE-UP GAS DRIERS (DR-2301/2302) (P&ID 023-PID-0021-011)
2.4 REGENERANT VAPORIZER (E-2305) (P&ID 023-PID-0021-012)

2.5 REGENERANT SUPERHEATER (A-2301) (P&ID 023-PID-0021-012)
2.6 FEED SURGE DRUM (D-2301) (P&ID 023-PID-0021-015)
2.7 REACTOR EXCHANGER CIRCUIT (P&IDs 023-PID-0021-015 to 018)
2.8 ISOMERIZATION REACTORS (R-2302/2303) (P&ID 023-PID-0021-019)
2.9 STABILIZER (T-2301) (P&IDs 023-PID-0021-020/021)
2.10 NET GAS SCRUBBER (T-2302) (P&IDs 023-PID-0021-022 to 026)
2.11 DE-ISOHEXANIZER (T-2303) (P&IDs 023-PID-0021-026 to 030)

1. PROCESS THEORY
1.1 PROCESS PRINCIPLES
The principle of the process is the isomerization reaction, which takes place in the
reactors. It is an equilibrium reaction and converts normal paraffins to isoparaffins, which
have a higher octane number.
Reaction takes place on a fixed bed catalyst, containing a supported noble metal and a
component to provide acidity. The reaction is operated in a hydrogen atmosphere and
employs perchloroethylene as a catalyst promoter, which is injected with the feed in the
range of concentration of 150 parts per million weight. The catalyst requires a dry, low
sulfur feedstock. Hydrocracking to light gases is generally slight.
The C5/C6 paraffin isomerization reactions, which occur in the Unit 023, are shown
below. The octane numbers presented in this section are for pure components:
NORMAL HEXANE 2 METHYL PENTANE

CH3
CH3 - CH2 - CH2 - CH2 - CH2 - CH3 ⇔ CH3 - CH - CH2 - CH2 - CH3
24.8 RON-O 73.4 RON-O
3 METHYL PENTANE
CH3
CH3 - CH2 - CH2 - CH2 - CH2 - CH3 ⇔ CH3 - CH2 - CH - CH2 - CH3
74.5 RON-O
2-2 DIMETHYL BUTANE

CH3
CH3 - CH2 - CH2 - CH2 - CH2 - CH3 ⇔ CH3 - C - CH2 - CH3
CH3
91.8 RON-O
2-3 DIMETHYL BUTANE

CH3
CH3 - CH2 - CH2 - CH2 - CH2 - CH3 ⇔ CH3 - CH - CH - CH3
CH3
104.3 RON-O
NORMAL PENTANE ISO PENTANE

CH3
CH3 - CH2 - CH2 - CH2 - CH3 ⇔ CH3 - CH - CH2 - CH3

61.8 RON-O 93.0 RON-O
2 METHYL PENTANE 2-2 DIMETHYL BUTANE

CH3 CH3
CH3 - CH - CH2 - CH2 - CH3 ⇔ CH3 - C - CH2 - CH3
CH3
2-3 DIMETHYL BUTANE

CH3 CH3
CH3 - CH - CH2 - CH2 - CH3 ⇔ CH3 - CH - CH - CH3
CH3
3 METHYL PENTANE 2-2 DIMETHYL BUTANE

CH3 CH3
CH3 - CH2 - CH - CH2 - CH3 ⇔ CH3 - C - CH2 - CH3
CH3
In the DIH, fractionation of the product occurs. In the following paragraphs, first, the
theory of the reaction and the history of the catalyst will be discussed, then the theory of
fractionation.
1.2 REACTION MECHANISMS
Paraffin isomerization catalysts fall mainly into either of two principal categories:
1. Those based on Friedel-Crafts catalysts as classically typified by aluminum
chloride/hydrogen chloride.
2. Dual-function hydro-isomerization catalysts.
The catalyst used in this isomerization unit is of the second category. For completeness
both mechanisms will be discussed.
1.2.1 FRIEDEL-CRAFTS CATALYST
No attempt is made to present a discussion of mechanisms of a degree of sophistication

acceptable to a chemist specializing in the area. The intention is simply to provide those
practicing engineers who have not previously had reason to consider isomerization with
a basic introduction to the subject.
Isomerization by either Friedel-Crafts or dual-function catalysts is generally thought to
entail intramolecular re-arrangements of carbonium ions as illustrated for pentane:
CH3
1. CH3 - CH - CH2 - CH2 - CH3 ⇔ CH3 - C - CH2 - CH3

⊕ ⊕
There appear to be two schools of thought regarding the Friedel-Crafts mechanism.
Perhaps each mechanism is operative and the disagreement is merely over their relative
importance under specific circumstances.
Friedel-Crafts isomerization is believed by some to require the presence of traces of
olefins or alkyl halides as carbonic ion initiators, with the reaction thereafter proceeding
through chain propagation. The initiator ion, which needs to be present in small amounts
only, may be formed by the addition of HCl or HAICI4 to an olefin, which is present in the
paraffin as an impurity or which is formed by cracking of the paraffin:
2. RCH = CH2 + HAICI4 → RCHCH3 + AICI4-
⊕
The initiator then forms a carbonic ion from the paraffin to be isomerized:
3. RCHCH3 + CH3-CH2-CH2-CH2-CH3 ⇔ RCH2CH3 + CH3-CH-CH2-CH2-CH3
⊕ ⊕
Skeletal re-arrangements then occur:

CH3

⊕ ⊕
Isopentane is then formed and the chain propagated by the generation of a new normal
carbonic ion:
CH3 CH3
5. CH3 - C - CH2 - CH3 + CH3 - CH2 - CH2 - CH2 - CH3 ⇔ CH3 - CH - CH2 - CH3 +
⊕ CH3 - CH - CH2 - CH2 - CH3
⊕
Naturally, the same sequence could have been illustrated starting with isopentane and
ending with n-pentane and an iso-carbonic ion to propagate the chain, i.e., reactions (3),
(4) and (5) are reversible, as are all of the reactions to be shown later. The composition
of the final mixture is, of course that set by thermo-dynamic equilibrium assuming that
sufficient reaction time has been provided.
Another Friedel-Crafts route, which has been suggested, is direct hydride ion
abstraction:
6. CH3 - CH2 - CH2 - CH2 - CH3 + AICI3 ⇔ CH3 - CH - CH2 - CH2 - CH3 + HAICI3-
⊕
The carbonic ion, as before, re-arranges:
CH3

⊕ ⊕
Finally, isopentane is formed:
CH3 CH3
8. CH3 - C - CH2 - CH3 + HAICI3- ⇔ CH3 - CH - CH2 - CH3 + AICI3

⊕
Abstraction of the hydride ion is energetically favored by the fact that the aluminum atom
can thereby complete its electron octet. Since there is always some hydrogen chloride
present, either by design or from hydrolysis of aluminum chloride by traces of water, a
Bronsted (protonic) acid could have been shown for Reactions (6) and (8) instead of a
Lewis acid:
9. CH3 - CH2 - CH2 - CH2 - CH3 + H+(AICI4)- ⇔ CH3 - CH - CH2 - CH2 - CH3 + (AICI4)- +
⊕ H2
Some chemists feel uncomfortable with the above because of the required postulation of
hydrogen formation.
1.2.2 DUAL-FUNCTION HYDRO-ISOMERIZATION CATALYST
The dual-function hydro-isomerization catalysts are thought by some to operate through

an olefin intermediate whose formation is catalyzed by the metallic component, assumed
for illustration purposes to be platinum:
Pt
10. CH3 - CH2 - CH2 - CH2 - CH3 ⇔ CH3 - CH2 - CH2 - CH = CH2 + H2
This reaction is, of course, reversible and, since these catalysts are employed under
substantial hydrogen pressure, the equilibrium is far to the left. However, the acid
function of the catalyst consumes the olefin by formation of a carbonic ion and thus
permits more olefin to form despite the unfavorable equilibrium. This step is entirely
analogous to Reaction (2) shown for Friedel-Crafts, except that it is better to denote the
acid function by a more general "H+A-".
11. CH3 - CH2 - CH2 - CH = CH2 + H+A- ⇔ CH3 - CH2 - CH2 - CH - CH3 + A-
⊕
The usual re-arrangements ensues:
CH3
12. CH3 - CH2 - CH2 - CH - CH3 ⇔ CH3 - CH2 - C - CH3

⊕ ⊕
The iso-olefin is then formed by the reverse analog of (11):
CH3 CH3
13. CH3 - CH2 - C - CH3 + A- ⇔ CH3 - CH2 - C = CH2 + H+A-

⊕
The iso-paraffin is finally created by hydrogenation:
CH3 CH3
Pt
14. CH3 - CH2 - C = CH2 + H2 ⇔ CH3 - CH2 - CH - CH3
Those dual-functional hydro-isomerization catalysts, which operate at very low

temperatures, have stronger acid sites than those, which require higher temperatures. In
this case it is possible that the necessary carbonic ion is formed by direct hydride ion
abstraction from the paraffin by the acid function of the catalyst:
15. CH3 - CH2 - CH2 - CH2 - CH3 + H+A- ⇔ CH3 - CH - CH2 - CH2 - CH3 + A- + H2
⊕
CH3

⊕ ⊕
CH3 CH3
17. CH3 - C - CH2 - CH3 + A- + H2 ⇔ CH3 - CH - CH2 - CH3 + H+A

The last reaction is in lieu of the displacement type chain propagation step, Reaction (5),
discussed earlier. Since the reaction with hydrogen is relatively fast, acid sites are readily
liberated for further reaction. This may account, at least in part, for the higher activity of
such dual functional catalysts.
1.3 HISTORY OF CATALYST
1.3.1 FRIEDEL-CRAFTS TYPE CATALYST
The isomerization catalysts employed during World War II were all of the Friedel-Crafts
type. Those, which contained aluminum chloride only, were either a
hydrocarbon/aluminum chloride complex (the so-called sludge process) or they were
manufactured in-situ by deposition onto a support such as alumina or bauxite. They were
intended to operate at very low temperatures (49°-129°C) and to approach the very
favorable equilibrium composition characteristics of these temperatures.
The catalyst tended to consume itself by reaction with the feedstock and/or product.
When temperature was raised a little in an effort to compensate for loss of catalyst and to
speed the reaction to effect more isomerization, light fragments were formed by cracking
and these, when vented, caused an excessive loss of the HCl promoter.
Corrosion of downstream equipment was also commonplace, due to the solubility of
aluminum chloride in hydrocarbon, to its relatively high volatility and to the difficulty of
removing it from the product by caustic washing. Aluminum chloride deposition in and
plugging of reboiler tubes was not uncommon.
The process faced problems in sludge disposal, which were considered onerous even
before the present acute awareness of environmental factors developed. The fixed bed
process sometimes experienced unpredictable amounts of isomerization.
1.3.2 HYDRO-ISOMERIZATION CATALYSTS ABOVE 200°C
The operational problems which had characterized the wartime Friedel-Crafts type
isomerization plants, the advent of catalytic reforming which not only made hydrogen
generally available in refineries but also demonstrated the practicality of using noble
metal containing catalysts on a large scale, and the octane number race which postwar
high compression engines initiated all combined in the 1950's to spawn a spate of hydro-
isomerization processes. These catalysts generally contained a noble metal and some
halide, operated at temperatures between about 299°C and temperatures approaching
those characteristics of catalytic reforming, employed recycle hydrogen to prevent
catalyst carbonization and utilized either no promoter or traces at most. In general, they
did not require an especially dry feedstock but did benefit from a low sulfur content
feedstock. Most achieved a close approach to the equilibrium characteristic of their
particular operating temperature.
Because of their high operating temperatures and their necessarily low conversions to
iso-paraffins, these high temperature catalysts were quickly replaced with the advent of
the "third generation" low temperature catalysts.
1.3.3 HYDRO-ISOMERIZATION CATALYSTS BELOW 200°C
"Low temperature" is considered rather arbitrarily for catalyst classification purposes as

anything below 200°C operating temperature. Typically these are fixed bed catalysts
containing a supported noble metal and a component to provide acidity in the catalytic
sense. They operate in a hydrogen atmosphere and may employ a catalyst promoter
whose concentration in the reactor may range from parts per million to substantially
higher levels. They generally all require a dry, low sulfur feedstock; however, they may
differ importantly in their tolerance of certain types and molecular weights of
hydrocarbons. Hydrocracking to light gases is generally slight, so liquid product yields
are high. As stated before, it is this type of catalyst that is used in the Isomerization Unit
023.
1.4 OTHER REACTIONS
Apart from the paraffin isomerization reactions which were discussed in detail in the
proceeding pages, there are several other important reactions including:
1. Naphthene ring opening
2. Naphthene isomerization
3. Benzene saturation
4. Hydrocracking
1.4.1 NAPHTENE RING OPENING
The three naphthenes, which are present in the feed of the isomerization unit, are
cyclopentane (CP), methyl cyclopentane (MCP) and cyclohexane (CH). The naphthene
rings will hydrogenate to form paraffins. This ring opening reaction increases with
increasing reactor temperature. At typical isomerization reactor conditions, the
conversion of naphthene rings to paraffins will be on the order of 20-40 percent.
1.4.2 NAPHTENE ISOMERIZATION
The naphthenes MCP and CH exist in equilibrium. Naphthene isomerization will shift
towards MCP production as temperature is increased.
METHYL CYCLOPENTANE CYCLOHEXANE
CH3
89.3 RON-O 84.0 RON-O

1.4.3 BENZENE SATURATION
The isomerization section is generally designed for 2 LV% benzene. The I-8 Plus and I-
82 catalysts will saturate benzene to cyclohexane. This reaction proceeds very quickly
and is achieved at very low temperatures. Saturation of benzene is not equilibrium
limited at the isomerization reactor conditions and conversion should be 100%. The
amount of heat generated by the saturation of benzene limits the amount of benzene,
which can be tolerated in the Penex, feed. The isomerization section feed can contain up
to 5% benzene. The platinum function on the isomerization catalyst is responsible for
benzene saturation.
BENZENE CYCLOHEXANE
+ 3H2
>100 RON-O 84.0 RON-O
1.4.4 HYDROCRACKING
Hydrocracking occurs in the Penex reactors to a degree, which depends on the feed quality
and severity of operation. Large molecules such as C7's tend to hydrocrack more easily
than smaller molecules. C5 and C6 paraffins will also hydrocrack to a certain extent. As
C5/C6 paraffin isomerization approaches equilibrium, the extent of hydrocracking
increases. If isomerization is pushed too hard, hydrocracking will reduce the liquid yield
and increase heat production. Methane, ethane, propane and butane are produced as a
result of hydrocracking.
NORMAL HEPTANE PROPANE + BUTANE
CH3
CH3 - CH2 - CH2 - CH2 - CH2 - CH2 - CH3 + H2 → CH3 - CH2 - CH3 + CH3 - CH - CH3
1.5 METHANATION
A methanator R-2301 is utilized for treating the makeup hydrogen gas of the isomerization
unit because of the catalyst extreme sensitivity to oxygenated compounds and H2S. Any
amount of CO, CO2 and H2S in the makeup hydrogen gas will affect the life of the catalyst.
The methanator can prolong the catalyst life by reducing the CO/CO2 concentration to low
ppm levels.
Moderately high levels of CO/CO2 can be produced in the continuous catalytic reformer unit
(U013). Even concentrations of 5-10 ppm CO/CO2 may be sufficient for justifying the
necessity of a methanator upstream of the reactors. Level traces of CO/CO2 will be removed
in the methanator through a nickel catalyst bed (PURASPEC 2443). The methanation of CO
occurs readily at 204°C, but the methanation of CO2 requires 316°C.
CO + 3H2 → CH4 + H2O + heat
CO2 + 4H2 → CH4 + 2H2O + heat
The methanation catalyst will also hydrogenate olefins and crack C2+ hydrocarbons. But it
can be permanently deactivated by sulfur. So, a preliminary catalyst bed (PURASPEC 2010)
will be used for H2S traces removal.
The water produced by the reactions will be removed in the makeup gas driers DR-
2301/2302.The methanation reaction is exothermic as are the side reactions, hydrogenation
and cracking. The methanation of feedstream with 1 mole percent of CO or 1 mole percent
CO2 can generate a delta T of hundreds of degrees. There is a danger of a temperature
excursion in circumstances where a sudden increase in CO/CO2 concentration can occur, or
where C2+ hydrocarbons, benzene or olefins can enter the methanator.
1.6 ACIDIZING
During the initial commissioning period, hydrogen chloride (HCl) is injected into the
process stream where it reacts with iron oxide (Fe2O3) to form iron chloride (FeCI3) and
water. This reaction will continue to take place until the rust present in the unit is
depleted. The absence of H2O in the unit, as detected by the moisture analyzers, will
signify that the reaction has gone to completion.
Hydrogen chloride + iron oxide → Iron chloride + water
6HCl + Fe2O3 → 2FeCI3 + 3H2O
1.7 CHLORIDE PROMOTER
The addition of the chloride promoter (perchloroethylene C2Cl4) to the process stream is
intended to maintain the acid function of the catalyst with chloride atoms (Cl). At a
reactor temperature of 105°C or higher, the organic chloride will decompose to HCl in the
presence of the I-8 Plus and I-82 catalysts.
Perchloroethylene + hydrogen → Hydrogen chloride + ethane
Catalyst
C2Cl4 + 5H2 → 4HCl + C2H6
Heat
1.8 CAUSTIC SCRUBBING
The hydrogen chloride formed in the isomerization reactors is neutralized in the Stabilizer
Net Gas Scrubber, by means of an acid-base reaction between sodium hydroxide
(NaOH) and hydrogen chloride (HCl). The result of this neutralization reaction is sodium
chloride (NaCl) and water. A diagram of the caustic scrubbing operation is shown in
Figure 2.1.1. The strength of the caustic should be monitored by determining the total
alkalinity of the solution. Report the concentration of strong base as wt% NaOH.
If a hydrogen stripping operation is performed, hydrogen sulfide (H2S) will be present in
the stabilizer off gas and will react with sodium hydroxide to form sodium sulfide (Na2S),
sodium bisulfide (NaHS) and water. During the sulfur stripping procedure it is important
to monitor the total alkalinity and the percent spent (the difference between the total
alkalinity and the strong base) as shown in Figure 2.1.2 and Figure 2.1.3. Report the
concentration of strong base as wt% NaOH.
HCl + NaOH → NaCl + H2O
H2S + 2NaOH → Na2S + 2H2O
H2S + Na2S → 2NaHS
HCl + Na2S → NaCl + NaHS
HCl + NaHS → NaCl + H2S
1.9 DE-ISOHEXANIZER (DIH): THEORY OF FRACTIONATION
At this point we will try to give the reader an understanding of how the various fractions
are separated in the DIH (T-2303).
It is well known that if water is heated to 100°C at atmospheric pressure, the water will
boil and steam vapors will rise from the surface of the liquid. It is equally well known that
if steam vapors are cooled they will condense to liquid water. The evaporation and
condensation of water are the fundamental principles underlying the production of
distilled water.
Now let us examine a mixture of alcohol and water and see how we can produce
essentially pure water and pure alcohol.
The alcohol will boil at approximately 60°C at atmospheric pressure; therefore, the
mixture of the two liquids will boil somewhere between 60°C and 100°C. The actual
boiling point will depend upon the composition of the mixture. The more alcohol that is
present, the lower will be the boiling point.
If this mixture is boiled, vapors made up of alcohol and water will be given off. Since
alcohol is the lighter compound in the mixture, there will be more alcohol, as a
percentage, in the vapors than in the liquid.
Let us now consider a mixture composed of 50% alcohol and 50% water. This mixture
will boil at about 79°C and will give off vapors consisting of, say 60% alcohol and 40%
water. If these vapors were condensed, and reboiled, the 60/40 mixture would boil at
about 77°C and give off vapors consisting of about 70% alcohol and 30% water. In this
manner, by successive vaporization and condensation, we would eventually obtain
almost pure alcohol boiling at about 60°C.
Likewise, the liquid remaining after the first vaporization would consist of only 40%
alcohol plus 60% water. This mixture would require a higher temperature of about 82°C
to produce vaporization. The vapors boiling from this mixture would consist of about 50%
alcohol and 50% water, leaving a liquid containing 30% alcohol and 70% water. Thus, by
successive reboiling and vaporizing off the lower-boiling alcohol, we would eventually
obtain substantially pure water boiling at 100°C.
It would require about six successive vaporizations and condensations between 79°C
and 60°C to produce almost pure alcohol. A further five reboilings of the liquid left after
the first vaporization, at temperatures between 79°C and 100°C, would result in the
production of almost pure water.
If all these steps were carried out separately, we would require 11 vessels, which would
make for a very uneconomical process. In practice, however, only one vessel would be
used and the 11 steps would be conducted on what are called "Fractionating trays".
These are just trays constructed in such a manner that a level of boiling liquid is
maintained on the tray while vapors from the tray below are bubbled through the liquid.
One type of fractionating tray used extensively in the past is one that is commonly called
a "bubble deck".
The vapors rise from the tray below and flow up through a number of risers in the tray
above. The bubble caps over each riser force the vapors into the liquid. The vapors then
flow through a number of slots on the side of the bubble cap and finally escape from the
liquid to rise to the next tray to repeat the process. The vapors coming from the tray
below will be cooled to the temperature of the liquid through which it bubbles. The vapors
that then rise from this tray will have a new composition, the actual composition
depending upon the temperature of the boiling liquid from which it leaves.
In the DIH of this isomerization unit sieve trays are used. The sieve tray is a flat
perforated plate. Vapor issues from the holes to give a multi orifice effect. The vapor
velocity keeps the liquid from flowing down through the holes. Sieve trays are simple and
therefore relatively inexpensive, but have a relatively poor turndown.
Now, if 11 of these fractionating trays were placed into one vessel, a "fractionating tower"
is produced that would fractionate or separate the alcohol and water. A sketch of the
fractionating tower for the alcohol/water separation is included to simplify the explanation
of the working of the tower. Some of the trays have been omitted to simplify the sketch
(Figure 2.1.4).
In order to have the column operate at its best, the 50/50 alcohol/water mixture is first
heated to its boiling point of 79°C and fed to the tower on the tray that is also operating at
79°C. If the alcohol/water mixture was fed in cold, it would upset the temperature
gradient through the tower by chilling the feed tray.
At the temperature of 79°C the vapors rising from the feed trays consist of 60% alcohol
and 40% water. The excess liquid from this tray flows down the downcomer to the trays
below and is composed of 40% alcohol and 60% water.
As the vapors from the feed tray rise through the liquid on the tray above they would
condense to form a liquid with a higher percentage water and a vapor containing a higher
percentage alcohol than the original vapor. The temperature of this tray is at the boiling
point of the liquid on the tray, so the vapors from this tray will consist of 70% alcohol and
30% water. The excess liquid from this trays will flow down the downcomer to the feed
tray. The vaporization and condensation will continue on up the column until we have
almost pure alcohol vapors leaving the top of the column at a temperature of 60°C. This
is referred to as "tower top temperature". The cooling of the tower from the 79°C feed
tray temperature to the 60°C top temperature is obtained by pumping back a portion of
the cooled and condensed overhead product to the top of the column. This stream is
called "reflux".
Meanwhile, the excess liquid from the feed tray is reboiled at a temperature of 82°C and
the vapors from this reboiling will consist of 50% alcohol and 50% water. The excess
liquid, 30% alcohol and 70% water, will flow to the tray below and will be reboiled at a
higher temperature. This will continue until the liquid is essentially pure water at the
bottom of the column. This is the "bottoms" and the temperature at which it leaves the
tower is the "bottoms temperature". The temperature rise between the feed tray at 79°C
and the bottoms temperature at 100°C is obtained by reboiling the bottoms product with
some outside source of heat. This source can be a circulating stream of hot oil (reboiler
oil), steam, or a gas or oil fired heater. By using 11 fractionating trays, a top reflux and a
bottom reboiler heat, we have separated the original 50/50 alcohol/water mixture into
alcohol and water. The whole process is referred to as "fractionation", "distillation" and
even "fractional distillation".
There are a few more points regarding fractionation that can be explained using the
foregoing illustration as an example.
The above discussion is mainly about the top reflux, but there is also an "internal reflux".
This is the excess liquid that flows from one tray down to the next. Using the feed tray as
an example and assuming some of the excess liquid can be removed as it flows to the
tray below and that the same quantity of reboiler heat is being added to the bottom of the
tower, there would be less liquid reaching the tray below the feed tray if some of the
internal reflux is removed. With less liquid flowing across this tray and the same amount
of heated vapors coming from the tray below, this tray temperature would increase and
can become 85°C instead of 82°C and less vapors would condense and more liquid
would vaporize, thus changing the equilibrium. The vapors leaving this tray now would
contain about 40% alcohol and 60% water instead of the previous 50/50 mixture. This
would change the liquid composition on the feed trays giving it a higher water content
than before and would require a higher tray temperature to boil this mixture. This would
also mean that the internal reflux leaving this tray would now have 65% water instead of
the 60% water it had before. Some of the internal reflux has been removed as a "side
cut". If we now increase this side cut, we will end up with a side cut having a water
content something greater than 65%.
If the rate at which the side cut product is withdrawn from the column is increased, there
will be less internal reflux available for the trays below. The tray temperature will increase
and a liquid of a heavier composition will be present on each of the trays and the side cut
product, still being taken from the same tray, will also be heavier.
The most important reflux stream, however, is still the top reflux. The amount of this
reflux will determine how good the fractionation will be between two compounds or two
fractions. If there is too much top reflux, there will be too much internal reflux. Each tray
will have a greater flow of liquid across it and the turbulence of the liquid on the tray will
increase. This will result in greater and greater liquid entrainment in the vapor as it
passes from one tray to the next. This liquid composition on each tray will change
because of this entrainment and the fractionation will no longer be a precise one. On the
other hand, too low a reflux will result in too little internal reflux resulting in a very low
flow of liquid across each tray. The contact between the rising vapors and the liquid on
each tray will not be as good. The vapors may not even have time enough to establish
an equilibrium with the liquid and less vapors will condense. The liquid composition on
each tray will change and again the fractionation will be a sloppy one.
The amount of reflux required to the top of a fractionating tower will depend upon the
quantity of the overhead vapors plus the quantity of heat to be removed from the top
portion of the tower. In order to increase the top reflux for better fractionation, it is usually
only necessary to increase the amount of heat that needs to be removed. This can
normally be done by increasing the quantity of reboiler heat applied to the bottom of the
column.
It would also be pertinent at this time to discuss the boiling point of a compound or of a
mixture. Each compound has its own vapor pressure, which is a measure of the
tendency of a molecule of the compound to escape from the liquid as a vapor. The vapor
pressure of a mixture is the sum of all the partial pressures of each compound in the
mixture. For example, in our 50/50 alcohol/water mixture, we could determine the vapor
pressure of the mixture by adding together 1/2 the vapor pressure of the alcohol plus 1/2
the vapor pressure of the water. The vapor pressure of this mixture would be midway
between the vapor pressure of the two compounds; hence, the boiling point will be
between the boiling points of the two compounds.
Analog to the alcohol/water example, the DIH fractionates the C5/C6 naphtha mixture that
is fed to the column.
The overhead consists of C5's and dimethyl butanes, the side draw is primarily
composed of methylpentane, some dimethyl butanes and nC6. The bottom stream is a
small flow, composed of the heavier boiling components, like cyclohexane and C7+.
Figure 2.1.1
Figure 2.1.2
Figure 2.1.3
Figure 2.1.4
This section will present a description of the flow through the isomerization unit, as well
as each major piece of equipment with its function and place in the process. Details
relating to operation will be discussed in Chapters 5 to 8.
For reference, Process Flow Diagrams of the Penex/DIH process unit are included in § 2
of Chapter 14. Further reference is made to the P&ID's of this unit: 023-PID-0021-
010/032.
2.1 FEED DRIERS (DR-2303/2304) (P&ID 023-PID-0021-013)
Hydrotreated light naphtha enters straightly the PENEX unit, and is first dried in the feed
driers DR-2303/2304.
The purpose of these driers is to ensure that the hydrotreated naphtha is dry before
entering the Reactors (R-2302/2303).
Indeed, due to the sensitivity of the I-8 Plus and I-82 reactors catalysts to water, the
feedstock must be routed through these molecular sieve driers. The driers are loaded
with UOP Molsiv Adsorbent HPG-250 for the removal of water and trace levels of
oxygenates or sulfur compounds.
The driers are operated in series except when they are in the regeneration mode. At that
time only one will be in service.
The hydrotreated C5/C6 stream is mixed with the recycle DIH side draw before being
introduced to the Feed Drier (DR-2303 or 2304) at the bottom and passes upflow
through the molecular sieve desiccant and exits at the top. The flow is then routed
through one of the drier crossovers to the other feed drier. The flow through the second
feed drier is also in the upflow pattern. The dried hydrocarbon is then routed to Feed
Surge Drum (D-2301). Over a period of time, the drier in the lead position will become
spent as indicated by the Moisture Analyzer (023-AT-001B) located between the two
driers. At this time, it will become necessary to regenerate this drier. The driers should be
regenerated on a schedule frequent enough to avoid moisture breakthrough. The spent
drier is taken out of service by closing the appropriate block valves. The second drier is
now alone in service as the only drier drying the feed. The moisture analyzer tap is
switched to monitor this in-service drier. After the drier regeneration has been completed,
it is now ready for service. A switch is made such that the regenerated drier takes the lag
position with the in-service drier remaining as the lead drier. Over a period of time the
lead drier will become spent and is now set up for regeneration with the tail drier now
being the only one in service. This will be the manner in which these driers will be lined
up for process flow. The regeneration procedure for the liquid driers is detailed in
Chapter 6.
The liquid feed driers are constructed from carbon steel and the hydrogen driers are
made from killed carbon steel. The bottom of the vessel is equipped with a carbon steel
outlet basket, covered with a steel mesh screen, to prevent loss of sieve or support
material. The molecular sieve and alumina are loaded between several layers of support
material. A holddown grating or screen is used on top of the sieve and the support
material to provide bed stability.
2.2 METHANATOR (R-2301) (P&ID 023-PID-0021-010)
Make-up gas is imported from the Make-Up Gas Knock-Out Drum / Lube Oil Mist
Eliminator (D-1208), downstream of the CCR Platforming Unit and Make-Up Gas
Compressor Section. It enters the Penex Process Unit at 42.3 kg/cm² (g) and 38 °C. It is
heated to 231 °C through the Methanator Feed / Effluent Exchanger (E-2301) and the
Methanator Heater (A-2302), then routed to the Methanator (R-2301).
The Methanator purpose is to protect the catalysts of the Reactors (R-2302/2303) from
trace levels of sulphur, CO or CO2 that could remain in the feed stream.
The Methanator is loaded with two catalysts dispatched on two superposed beds with the
feed passing down flow:
Puraspec 2010 for sulphur absorption (upper bed)
Puraspec 2443 for methanation (lower bed)
The catalysts are loaded between a graduated system of inert ceramic balls.
The water produced during the methanation reaction and any CO2 not methanated will
be removed in the Make-up Gas Driers DR-2301/2302.
The treated gas is cooled through the Methanator Feed / Effluent Exchanger E-2301 and
the Methanator Cooler E-2303. It enters the Make-Up Gas Driers at 38°C and 37.4
kg/cm² (g).
2.3 MAKE-UP GAS DRIERS (DR-2301/2302) (P&ID 023-PID-0021-011)
Make-up gas must be dried in order to protect the I-8 Plus and I-82 catalysts for the
same reason as described at the feed drier section. The make-up gas driers are loaded
with UOP Molsiv Adsorbent PDG-418, a molecular sieve for the removal of water.
The two gas driers operate in the same manner as the feed driers. The driers operate
upflow, in series. The dried hydrogen is then sent to the reactor circuit on Flow Control
(023-FIC-013). The hydrogen is also used for pressure control (023-PIC-090) in the Feed
Surge Drum (D-2301) and, for start-up, in the Stabilizer (T-2301). The regeneration
procedure for the gas driers is detailed in Chapter 6.
The make-up gas driers are made from killed carbon steel. The design of the drums is
similar to the feed driers one.
2.4 REGENERANT VAPORIZER (E-2305) (P&ID 023-PID-0021-012)
The regenerant vaporizer uses low pressure steam to heat the regenerant stream before
it reaches the electric superheater. The vaporizer, shown in Figure 2.2.2, is an upright
heat exchanger which uses bayonet type tubes that have been strength welded and fully
rolled. This heater is equipped with a level indicator and a high level alarm, and is
designed to operate with the top portion of the tubes uncovered. Low pressure steam on
the inside of the bayonet tubes transfers heat to the regenerant on the outside of the
bayonet tubes. This arrangement allows hot steam in the tip of the bayonet tube to
transfer heat to the vaporized regenerant stream to 119-120°C, giving it several degrees
of superheat. This prevents the regenerant from condensing which could damage the
electric bundles in the regenerant superheater (A-2301) when operating. The liquid level
in the vaporizer is available from 023–LI-003. 023-LXAHH-004 in E-2305 will trip the
regenerant superheater A-2301.
2.5 REGENERANT SUPERHEATER (A-2301) (P&ID 023-PID-0021-012)
The regenerant superheater, shown in Figure 2.2.3, raises the temperature of the
vaporized regenerant to a temperature of 316°C. The regenerant stream is heated by
Inconel electric elements, which are capable of reaching temperatures of over 600°C.
The regenerant entering the superheater must be in the vapor phase to avoid damaging
the electric bundles when power is applied to the superheater.
2.6 FEED SURGE DRUM (D-2301) (P&ID 023-PID-0021-015)
The liquid feed from the liquid feed driers is routed to the Feed Surge Drum (D-2301).
The purpose of this drum is to provide liquid feed surge capacity for the downstream
process. The feed surge drum is blanketed with dry hydrogen gas originating from the
outlet of the Make-up Gas Driers (DR-2301/2302) with the feed surge drum pressure
being controlled by 023-PIC-090 at 6.2 kg/cm² (g). The vessel is constructed of killed
carbon steel.
2.7 REACTOR EXCHANGER CIRCUIT (P&IDS 023-PID-0021-015 TO 018)
The dried liquid feed from the feed surge drum (D-2301) is pumped by either of the two
Charge Pumps (P-2301 A/B) through the reactor exchanger circuit on Flow Control (023-
FIC-009). The reactor exchanger circuit consists of the Cold Combined Feed Exchanger
(E-2306), the Hot Combined Feed Exchangers (E-2307 A/B) and the Charge Heater (E-
2308).
The Heat Exchangers E-2306 and E-2307 A and B are combined reactor feed/reactor
effluent shell and tube exchangers. The charge heater (E-2308) uses MP steam. Because
the hydrocarbon stream has to be totally dry, the charge heater operates with pressure of
hydrocarbon higher than the pressure of the steam. The exchanger utilizes strength
welded and fully rolled tube sheets in order to minimize the potential for leakage (see
Figure 2.2.1).
Prior to the entry into the cold combined feed exchanger (E-2306), the liquid hydrocarbon
is combined with the make-up hydrogen stream. After combining, the mixed
hydrocarbon-hydrogen stream passes through the exchanger circuit in the order
previously mentioned E-2306, E-2307 B, E-2307 A and E-2308 shell side. Under normal
operation reactor feed enters the reactor at a pressure of about 35 kg/cm² (g) and a
temperature between 133°C and 162°C.
The cold combined feed exchanger (E-2306) is equipped with a bypass which can be
used to regulate the amount of combined feed preheat to 38-112°C. The bypass is
manually regulated with Control Valves (023–HV-006 A/B) to maintain reactor charge
heater control. The combined feed is further preheated by exchange with a portion of the
lead reactor effluent in the hot combined feed exchangers (E-2307 A/B) to 123-151°C,
regulated by 023-TV-024 A/B.
A small quantity of catalyst promoter (perchloroethylene) is added upstream of the
reactor charge heater. This promoter is pumped into the process by either of the two
Chloride Injection Pumps (P-2303 A/B). The catalyst promoter is stored in a nitrogen
blanketed storage drum (Chloride Injection Drum, D-2302) at 1.76 kg/cm² (g) and 38°C.
The storage drum is filled with perchloroethylene, which is transported to site in drums.
These drums can be connected to the process. From the drums the catalyst promoter is
pumped with the Chloride Transfer Pump (P-2302 A) into the Chloride Injection Drum (D-
2302).
The combined feed is finally brought up to the desired temperature of 133-162°C in the
reactor charge heater (E-2308) by a Temperature Controller (023-TIC-056) which resets
the exchangers heating medium flow. The charge heater is equipped with an automatic
shutdown, which is activated by low feed or low make-up gas flow.
After exiting the reactor charge heater, the heated combined stream then flows to the
first reactor.
2.8 ISOMERIZATION REACTORS (R-2302/2303) (P&ID 023-PID-0021-019)
The reactors R-2302 and R-2303 are the heart of the process. The operation of them is
such that a reactor will be placed in series with the other reactor. At various times
throughout the unit's history it will be possible to have either reactor in the lead or tail
position. A single reactor bypass allows operation of one reactor only during start-up or
partial catalyst replacement. Thermocouples are inserted into the isomerization catalyst
bed of each reactor to monitor the activity of the catalyst in conjunction with product
ratios.
Reactor R-2302 is loaded with I-8 Plus catalyst and reactor R-2303 is loaded with I-82
catalyst.
After exiting the reactor charge heater, the heated combined stream then flows to the
first reactor, the lead reactor. The feed/hydrogen mixture enters the reactor vessel top
through an inlet distributor and leaves at the bottom. There is a vapor/liquid distributor
tray installed above the I-8 Plus and I-82 catalyst beds to assure even distribution (see
Figure 2.2.4). The bottom head of the reactor has a screen basket that allows the
process stream to pass through it, but prevents any ceramic support material to migrate
downstream into the unit. The vessels are constructed of killed carbon steel. Upon
exiting the first reactor, the stream then passes to the hot combined feed exchanger (E-
2307 A/B) at 182-188°C where the first reactor's heat of reaction is partially removed and
cooled down to 112-155°C.
The degree of temperature removal can be achieved by adjusting the amount of
exchanger by-passing with a Temperature Controller (023-TIC-024). This temperature
controller fixes the lag reactor's inlet temperature.
The partially cooled stream is then routed to the second reactor, the lag reactor, where
the final process reactions are completed
The reactors are equipped with hydrogen purge line (1½”-PG-230154-B1AH-NI), which
is located at the inlet of each reactor. The hydrogen purge is used to remove
hydrocarbon from a reactor which is to be unloaded or to pressurize a reactor. A
hydrogen quench line (3”-PG-230131-B1AH-NI) is located at the lead reactor inlet
header to aid in cooling the catalyst during a temperature excursion as well as removing
hydrocarbon. The quench is controlled by 023-HIC-012 with flow indication (023-FI-015).
The reactors are equipped with a depressuring line to the flare system (3”-PZ-230161-
B1AH-NI). In case of high reactor temperature emergency the reactors are depressured
from the outlet of the lag reactor. The depressuring line is equipped with two
pneumatically operated Valves (023-XV-093 A and B) which can be operated from the
control room once the reactors have been isolated from the charge heater and stabilizer.
After exiting the second reactor, the stream is then routed to the tube side of the cold
combined Feed Exchanger (E-2306) to be cooled down to 115°C.
The cold combined feed exchanger tube side effluent is then routed to the Stabilizer (T-
2301) on Pressure Control (023-PIC-097).
2.9 STABILIZER (T-2301) (P&IDS 023-PID-0021-020/021)
Feed to the stabilizer enters at a pressure of 15.9 kg/cm² (g) and a temperature of
113°C.
The purpose of this column is to separate any dissolved hydrogen, HCl and cracked
gases (C1, C2 and C3’s) from the isomerate, which is the product coming of the
isomerization unit.
The isomerate is the bottom stream of T-2301. It is at 175-176°C and 15.0 kg/cm² (g)
and contains normal and isoparaffins and is sent to the de-isohexanizer (DIH, T-2303)
column on Level Control (023-LC-007). Prior to entering the DIH, the stabilizer bottoms
stream exchanges heat in the deisohexanizer side draw reboiler (E-2312) to be cooled
down to 132-133°C.
The stabilizer column overhead vapor at about 79°C and 14.8 kg/cm² (g), consisting of
the light hydrocarbon components of the column's feed, is routed to the air cooled
Stabilizer Condenser (E-2310) to be condensed and cooled to 50°C and then, via the
Stabilizer Trim Condenser (E-2311) (to be cooled to 38°C) to the Stabilizer Receiver (D-
2303). To maintain pressure control on the column at 14.8 kg/cm² (g), gas is vented on
Pressure Control (023-PIC-022) to the Net Gas Scrubber (T-2302). Liquid is pumped
from the receiver on Level Control (023-LIC-008) with one of the Stabilizer Reflux Pumps
(P-2304 A/B). All liquid from the stabilizer overhead receiver is refluxed to the stabilizer
column on Tray No. 1.
The column is reboiled by MP steam in Stabilizer Reboiler (E-2309). The reboiler heat
input is controlled by 023-FIC-016 on the MP condensate outlet of the reboiler. The
amount of heat input is adjusted to maintain sufficient reflux to adequately strip the HCl
and light ends from the stabilizer bottoms material. The typical design external reflux to
feed ratio is approximately 0.5 on a volume basis and is recommended as a starting
point.
The top half of the stabilizer is narrower than the bottom half because of the smaller
amount of vapor/liquid traffic that occurs in the top part of the column. The stabilizer feed
enters through a distributor located at the bottom of the conical section between tray 15
and 16. A liquid trap is placed below tray 15 in order to create a liquid seal in the tray
downcomer and thus preventing the vapor from bypassing this tray.
2.10 NET GAS SCRUBBER (T-2302) (P&IDS 023-PID-0021-022 TO 026)
The function of the stabilizer Net Gas Scrubber is to neutralize the hydrogen chloride
present in the stabilizer off gas prior to its entry into the fuel gas system. The HCl is
formed in the reactor section and then vented off through the Stabilizer Overhead
Receiver (D-2303), to the Stabilizer Net Gas Scrubber (T-2302). In this vessel, the off
gas from the stabilizer receiver is contacted through a liquid level and later with a counter
current flow of caustic solution (10 wt% NaOH) which reacts with HCl to form sodium
chloride and water. The column operates at 6.3 kg/cm² (g) and 38°C. The entry point for
the off gas is located at the bottom of the scrubber, and consists of a Monel distributor
with small holes to allow even gas distribution. The bottom distributor and the inlet flange
are both made of Monel to prevent corrosion, resulting from contact with high
concentrations of HCl in an aqueous environment. The vessel is constructed of killed
carbon steel.
Two packed beds, installed in the top portion of the vessel, are filled with 19 mm Carbon
Raschig Rings, which provide a good contact area for the interaction of the liquid phases
and the acidic overhead gas. The packings in the scrubbing section are held in place by
a support grating on the bottom and a hold down grating on the top.
The incoming gas is contacted with the caustic in the bottom portion of the scrubber (or
"reservoir" section) through the packed bed number 2. This is where most of the HCl is
removed before it reaches the top portion or the scrubbing section of the column. The
caustic level in the scrubber is maintained about 0.3-0.6 m below the distributor under
the packed section. Pump P-2307 A or B (Caustic Circulation Pumps) is used to circulate
the caustic to the two injection points on the scrubber column. One injection point is
located between the two packed beds and the other is located just below the packed bed
number 2 (spray nozzle distributor). The purpose of the lower spray distributor is to direct
the caustic flow to the conical walls of the scrubber to keep the walls wetted with caustic.
The design flow of caustic should be continuously maintained to each distributor to
ensure good flow distribution.
Periodically (about once a week) a portion of the caustic is withdrawn as spent caustic to
Caustic Degassing Drum D-2305, then Spent Caustic Neutralisation Package X-2399.
Fresh 14.4 wt% caustic is imported from Unit 039 and diluted down to 10 wt% with make-
up water from Water Break Tank (D-2304). Caustic strength should not fall below 2 wt%
NaOH.
On the top part of the column, the gas is washed with water through the packed bed
number 1 in order to remove entrained caustic. P-2308 A or B (Water Circulation Pump)
is used to circulate the wash water to the injection point at the top of the packed section.
Cold Boiler Feed Water, cooled down to 38°C through the Condensate Cooler E-2319, is
used for make-up. Make-up injection into the system is carried out by mean of the Water
Injection Package X-2304, composed of the Water Break Tank D-2304 and Water
Injection Pumps P-2309 A/B.
The scrubbed gas leaves the top of the column and is directed as net gas to the Refinery
Fuel Gas Unit 037 on Pressure Control (023-PIC-024) at 37°C and 4 kg/cm² (g). The
hydrogen purity of the net gas is monitored with 023-AI-003 in order to determine the
hydrogen-hydrocarbon ratio (see § 3 of Chapter 3).
2.11 DE-ISOHEXANIZER (T-2303) (P&IDS 023-PID-0021-026 TO 030)
The DIH is used to recover pentanes and product isohexane from the stabilized reactor
products. A side draw, composed primarily of methylpentanes, 2,3-DMB and n-hexane,
is recycled back to the liquid Feed Driers (DR-2303/2304).
A typical isomerization unit can upgrade light straight run naphtha from 70.0 RONC to
82.0-84.0 RONC. However, there is a significant amount of C6 isomers that can be
further upgraded to 2,2-DMB. The overhead product from the DIH has the potential to
have an octane value of 88.0-90.0 RONC.
The DIH has 80 trays. The column operates at 1.32 kg/cm² (g) and a volumic reflux/feed
ratio of about 3.0. Feed from the bottom of the stabilizer (T-2301) exchanges heat with
the DIH column side draw effluent in the Deisohexanizer Side Draw Reboiler (E-2312)
before entering the column on Tray No. 25 at 132°C and 2.15 kg/cm² (g).
The bottom product is pumped by the De-isohexanizer Bottoms Pumps (P-2311 A/B) and
cooled by the De-isohexanizer Bottoms Cooler (E-2315) before sending to storage.
Overhead vapor from the DIH at 72°C and 1.3 kg/cm² (g) is condensed via the air cooler
E-2317 A/D (De-isohexanizer Condenser) to 56°C and 0.7 kg/cm² (g) and the liquid
accumulates in the Deisohexanizer Receiver (D-2306). The receiver serves as a reflux
drum.
Liquid of the Deisohexanizer Receiver (D-2306) is pumped by Deisohexanizer Overhead
Pumps (P-2312 A/B). A large portion (60%+) of the overhead liquid is sent back to the
top of the DIH on flow control (023-FIC-031). Level controller 023-LIC-015 will act when
the level vary, by resetting the flow controller set point. The net overhead flow is on
compositional control via Upper Tray Temperature Control (023-TIC-047), cascaded to
Net Overhead Draw Flow Control (023-FIC-031). Upper Tray Temperature Control can
be overridden by DIH side draw process gas chromatograph (023-AT-004) or DIH
overhead process gas chromatograph (023-AT-005) if one of the chromatograph set
point is reached.
Before sending to tankage or gasoline blending, the net overhead stream is further
cooled by the Isomerate Cooler (E-2318).
A part of the isomerate is used for the regeneration of both feed driers (DR-2303/2304) and
make-up gas driers (DR-2301/2302). After service in the driers, the product joins the
bottom material, which is sent to storage.
A side draw containing products with a low octane grade is pumped by Deisohexanizer
Side Draw Pumps P-2310 A/B, cooled down to 38°C through Deisohexanizer Side Draw
Air Cooler E-2313 and Water Cooler E-2314 before being sent back to the Feed Driers
DR-2303/2304 to be retreated in the Isomerization reactors R-2302/2303. Upstream of
the Deisohexanizer Side Draw Pumps, a part of the side draw flow is sent to the
Deisohexanizer Side Draw Reboiler E-2312 where it exchanges heat with Feed from
104-106°C to 109-111°C, before being sent back to the Deisohexanizer column.
The DIH column operation is fairly straightforward. The basic guidelines are to remove all
the pentanes and 2,2-DMB overhead, while minimizing the 3 methylpentane content in
the overhead.
The way of control is discussed in the following (refer to 8474L-023-PID-0021-026 thru
030 attached in § 2 of Chapter 14).
For many years, the "conventional" composition control system was used to control
simple two product fractionators such as a DIH. That is, fixing the pressure and heat
input, having the receiver level control the net overhead product flow and using the
composition control (typically a column tray temperature) to adjust the reflux flow rate. In
the late 1960's, articles were published that suggested that there may be a better way to
control this type of column. This alternate scheme has been discussed in a number of
texts and is commonly known as the "material balance" or "flywheel" control scheme.
The basic difference between "conventional" and "material balance" control schemes is
in the choice of variables used to alter the column reflux flow. The pressure and heat
input controls remain the same. In the material balance control scheme, the reflux flow
rate is controlled by the level in the overhead receiver. The column compositional control
(tray temperature) is then connected to adjust the net overhead liquid flow leaving the
receiver. This concept led to the term "flywheel" control where the heat balance creates a
mechanism for separation by developing a circulation of material, vapor rising and liquid
refluxing analogous to the momentum of a flywheel. The composition control directs the
correct amount of product out of the top of the column and by material balance, out of the
bottom. If the composition sensor is not satisfied, it will not allow the overhead product to
leave the receiver. The level in the receiver will rise causing the products to be returned
to the column resulting in an increase in reflux rate which improves separation and
returns the composition sensor to its desired value.
It is fairly apparent that the level control on the receiver is very important to the operation
of the material balance control scheme since it is the intersection point for the material
and energy balances in the column. When the composition controller asks for a change
in the rate of net overhead liquid, the result will be a change in the rate of reflux after the
level controller has sensed a change in the receiver level. For this reason, the material
balance control scheme required a high gain on the receiver level controller so that the
control system would be quick at sensing changes and act on them. In practice, the level
controller gain setting desired was sometimes not feasible due to problems with the
receiver's capacity or level instrument conditions. As a result, the system was changed to
a variation on the material balance scheme, which we call the modified flywheel control
scheme.
The modified flywheel control scheme is similar to the material balance approach.
However, the Reflux Flow Controller (023-FIC-034) is now the sum of product flow and
reflux flow, and as such, can be assimilated as a total overhead liquid flow meter. By
doing this, any changes the composition control requires in the net overhead liquid flow
are immediately sensed by the total overhead flow meter and an equivalent change is
made in the reflux flow rate. This eliminates the need for an extremely "hot" Level
Controller (023-LIC-015) on the receiver as it now only needs to correct the total
overhead liquid flow due to changes in the column heat balance. The Net Overhead Flow
Meter (023-FIC-031) simply routes the composition controlled amount of material from
the column and the balance of the total overhead liquid is returned to the column as
reflux.
In a sense, this system allows the composition controller to adjust both the heat and
material balances at the same time, due to the close interaction between the two flow
controllers. This is reflected in actual operating experience of seeing only slight changes
to the total overhead rate and receiver level (intersection of the two balances) during
changes in the column's operation.
Another difference with the flywheel control is the column composition control: the
overhead product is still sent to storage on flow control (023-FIC-031) reset by column
tray temperature control (023-TIC-047). If temperature is above set point, the
temperature controller will reduce set point of 023-FIC-031 and then reduce the net
overhead flow.
However, two chromatograph analyzers have been added to control side draw and
overhead compositions.
The first one (023-AT-004 A/B) analyzes the 2,2 Dimethylbutane and 2,3 Dimethylbutane
amount in the side straw stream. Its purpose is to minimize the light compounds on side
cut and obtain the best performance from the isomerisation reactor section.
The second one (023-AT-005 A/B) analyzes the 2-Methylpentane and 3-Methylpentane
amount in overhead stream in order to control the correct amount of net overhead
product.
Both of them are linked to the Analyzer Calculator 023-AY-005B. If one of the
composition sensor is not satisfied, 023-AY-005B will override tray temperature controller
and become the remote setpoint to the net overhead flow controller, by mean of the
switch 023-HS-015.
The DIH overhead pressure control is via a totally condensing hot vapor bypass control
system. The flow to the overhead condenser is controlled by 023-PIC-027, while the
pressure differential across the condensers and 023-PV-027 is set by the hot vapor
bypass. The hot vapor from the bypass heats the top layer of liquid in the receiver, which
in turn raises the vapor pressure in the receiver. 023-PDIC-028 is adjusted so 023-PV-
027 can stay in a controllable range. Lines for venting of the condenser and receiver are
provided for start-up and, if necessary, normal operations due to possible accumulation
of non-condensable build-up.
Heat is provided to the DIH via the Side Draw Reboiler (E-2312), exchanging heat with
the feed stream, and a Reboiler (E-2316) using medium pressure steam.
The side draw reboiler flow is controlled via the side draw outlet tray level controller 023-
LIC-013. The heat input of the side draw reboiler is calculated by mean of the Heat Input
Calculator 023-XY-005 and sent to DCS.
For the steam reboiler, heat input is controlled on the condensate side. The condensate
is flow controlled from the reboiler via 023-FIC-026. The reboiler heat input is adjusted to
maintain the proper reflux to feed ratio, while keeping the overhead methylpentane
content at its normal level.
The bottoms product from the column is a small flow. It is yielded on Flow Control (023-
FIC-028).
The DIH recycle stream is taken off as a lower side cut. The lower side cut is pumped
back by either of Side Draw Pumps (P-2310 A or B), cooled down to 38°C through Side
Draw Air Cooler (E-2313) and Side Draw Water Cooler (E-2314), then sent to the liquid
feed driers on flow control (023-FIC-030). The flow controller is reset by the Level
Controller (023-LIC-014) of the column.
The heavies in the side draw should be minimized for best performance of the reactors.
The majority of cyclo-hexane and C7+ material should be rejected out the bottom of the
tower. As the amount of heavies in the side draw increases, the operator should increase
the net bottom flow.
The net bottoms product at about 136°C is pumped out by De-isohexanizer Bottoms
Pump (P-2311 A or B) via the DIH Bottoms Cooler (E-2315) where it is cooled to 37°C
and then mixed with the overhead product stream to storage.
The octane of the overhead product is set by two independent variables:

1. The pentane composition of the overhead.
The total amount of pentane in this stream is set by the feedstock composition. The
isopentane content is then set by the degree of C5 isomerization in the reactors. For a
given feedstock composition, the octane of the overhead is improved by maximizing
the IC5/C5P ratio in the overhead product. Since the pentanes in the product are
processed "once-through", the higher the concentration of pentanes in the feedstock,
the lower the product octane will be.
2. The amount of 2-methylpentane and 3-methylpentane in the overhead.
Since these components have an octane blending value of about 75, the higher their
concentration in the overhead product, the lower the octane will be. Since eliminating
all of the methylpentanes would required; a) more trays, b) more reflux and c) more
recycle to the reactor section, an economic compromise must be made to adjust the
product octane vs. utility consumption.
Generally, about 80% of the methylpentanes are recovered in the recycle stream back to
the reactor section. If a higher octane product is required then the tower reflux should be
increased, the overhead rate decreased and the liquid recycle to the liquid feed driers
increased.
Figure 2.2 .1
Figure 2.2 .2
Figure 2.2 .3
Figure 2.2 .4
CHAPTER 3
DESCRIPTION OF PLANT CONTROL
CONTENTS
1.1 FEED SURGE DRUM (D-2301) PRESSURE CONTROL
1.2 REACTOR AND ITS EXCHANGER CIRCUIT
1.3 DEISOHEXANIZER (T-2303)

1.3.1 OBJECTIVE
1.3.2 PRESSURE CONTROL
1.3.3 OVERHEAD TEMPERATURE AND REFLUX LIQUID CONTROL
1.3.4 SIDE DRAW FLOW AND COLUMN BOTTOM LEVEL CONTROL
1.3.5 REBOILER HEAT INPUT CONTROL
3.1 PROCESS VARIABLES OF THE REACTOR SECTION

3.1.1 REACTOR TEMPERATURE
3.1.2 LIQUID HOURLY SPACE VELOCITY
3.1.3 HYDROGEN TO HYDROCARBON MOL RATIO
3.1.4 PRESSURE
3.1.5 CATALYST PROMOTER
3.1.6 PROCESS CONTAMINANTS
3.2 PROCESS VARIABLES OF DIH

3.2.1 FEED COMPOSITION
3.2.2 PRESSURE
3.2.3 INLET TEMPERATURE
3.2.4 REFLUX/FEED RATIO
3.2.5 REBOILERS HEAT INPUT
3.2.6 SIDE DRAW RATE
3.2.7 SIDE DRAW TRAY TEMPERATURE


1.1 FEED SURGE DRUM (D-2301) PRESSURE CONTROL
PID reference: 8474L-023-PID-0021-015

The purpose is to control the drum blanketing pressure by mean of a split range pressure
controller PIC-090 operating on control valve PV-090A in H2 gas import line (0-50%) or
control valve PV-090B in the off-gas bent line to the flare (50-100%). In case of pressure
lower than setpoint, PV-090A will open while PV-090B remains close. In case of pressure
higher than setpoint, PV-090B will open while PV-090A remains close.
1.2 REACTOR AND ITS EXCHANGER CIRCUIT

8474L-023-PID-0021-018
8474L-023-PID-0021-019
Reactor temperature is the main process control in this section. Penex unit has two series
reactors with provision for independent temperature control. The first reactor will be
operated at such a temperature as to maximize the concentration of Isopentane in its
effluent. The required temperature in 2nd reactor is reduced.
Prior to the entry of the liquid feed, which on flow control FIC-009, into the cold combined
feed exchanger, it combines with the makeup H2 stream on flow control FIC-013. H2 is
maintained high enough for reaction H2/HC ratio, which is determined by means of FFY-051.
The cold combined feed exchanger is equipped with a bypass control HIC-006, which
can be used to regulate the amount of combined feed preheat. In case of temperature
lower than setpoint, HV-006A will open while HV-006B will close. In case of temperature
higher than setpoint, HV-006B will open (0-100%) while HV-006A will close (100-0%)
accordingly.
The combined feed is further preheated by exchange with a portion of the LEAD reactor
effluent in the hot combined feed exchanger. The degree of temperature gain can be
achieved by adjusting the amount of exchanger by passing with a temperature controller
TIC-024 using split range. TIC-024 adjusts control valve TV-024B in the bypass line of heat
exchanger E-2307A/B (0-100%) and control valve TV-024A in the main line to the LAG
reactor (100-0%). This temperature controller fixes the LAG reactor’s inlet temperature.
The combined feed is finally brought up to the desired temperature in the reactor charge
heater by a temperature controller TIC-056, which resets the exchangers heating medium
flow control FIC-014.
After exiting the reactor charge heater, the heated combined stream then flows to the first
reactor. A H2 quench line is located at the lead reactor inlet to aid in cooling the catalyst
during a temperature excursion. The quench is controlled by an HIC-012 with flow indicator.
After exiting the second reactor, the stream is routed to stabilizer on pressure control PIC-
097.
1.3 DEISOHEXANIZER (T-2303)

8474L-023-PID-0021-027
8474L-023-PID-0021-028
8474L-023-PID-0021-029
8474L-023-PID-0021-030
1.3.1 OBJECTIVE
The purpose of deisohexanizer is to recover product isohexane and pentanes from the
stabilized reactor products. A sidedraw, composed primarily of methypentanes, 23-DMB and
n-hexane, is recycled back to the Isomerization unit for further upgrading. Stabilizer bottoms
is fed to the deisohexanizer on level control LIC-007.
1.3.2 PRESSURE CONTROL

Good column operation requires that pressure be held stable. The DIH overhead pressure
control is via a totally condensing hot vapour bypass control system. The flow to the
overhead condenser is controlled by PIC-027, while the pressure differential controller
PDIC-028 across the condensers. The hot vapour from the bypass heats the top layer of
liquid in the receiver, which in turn raises the vapour pressure in the receiver. The PDIC-028
is adjusted so that the PV-027 can stay in a controllable range.
1.3.3 OVERHEAD TEMPERATURE AND REFLUX LIQUID CONTROL

The overhead product is sent to storage on flow control FIC-031 reset by column tray
temperature control TIC-047. In case measured temperature is above setpoint, TIC-047 will
reduce setpoint of FIC-031, which will in turn reduce the opening of FV-031. As overhead
product flow decrease, the measure to FIC-034 will decrease, as it is the sum of product
and reflux FY-033 (calculated from FT-031 and FT-033). The consequence will be that FIC-
034 output will increase to compensate this loss and more reflux will be sent to the column
T-2303 to maintain an equal draw flowrate from D-2306. This will allow level of D-2306 to
maintain constant despite product draw being reduced.
The level controller LIC-015 will act when level vary. In case level is increasing above
setpoint, the setpoint of FIC-034 will be increased. As overhead product flow measurement
remains the same, the consequence will be that FV-034 will open more to increase reflux
flow to T-2303.
By means of compositional control AIC-005A/B (chromatograph) the correct amount of net
overhead product will be controlled through the switch HS-015. If the composition sensor is
not satisfied, it will not allow the overhead product to leave the receiver. The level in receiver
will rise causing the products to be returned to the column resulting in an increase in reflux
rate which improves separation and returns the composition sensor to its desired value.
1.3.4 SIDE DRAW FLOW AND COLUMN BOTTOM LEVEL CONTROL

The heavies on the sidecut will be minimized to obtain the best performance from the
isomerization reactor section by means of composional control AIC-004A/B. The side cut
is pumped back to isomerization unit on flow control FIC-030. The flow control is
cascaded from the column bottom level control LIC-014. The bottom flow to storage is a
small flow. It is yielded from the column on flow control FIC-028.
DIH FEED Services as side draw reboiler by means of Heat exchanger E-2312. The heat
Input will be calculated through TI-043, TI-044, FI-024 and XY-005.
1.3.5 REBOILER HEAT INPUT CONTROL

Heat is provided to the DIH via a thermosyphon reboiler (E-2316) using desuperheated MP
steam by condensate flow control FIC-026. The reboiler heat input is adjusted to maintain
the proper reflux to feed ratio.
Refer to the Process Flow Diagrams 8474L-023-PFD-0010-001 thru 005 included in
section § 2 of Chapter 14.
This paragraph is split into two parts. In the first section, the variables of operation of the
Penex reactors will be discussed. The second part is for the discussion of the principal
process variables of the de-isohexanizer column.
3.1 PROCESS VARIABLES OF THE REACTOR SECTION

In the normal operation of the isomerization unit, having once set the operating pressure,
fresh feed rate and make-up hydrogen flows, it is usually only necessary to adjust the
reactor inlet temperatures. Nevertheless, it is to the operator's advantage that he has a
thorough understanding of the influence process variables will have on performance of
the unit and the life of the catalyst.
Once the catalyst has been loaded into the reactors, the manner in which the catalyst is
placed in service and the treatment it receives when in service will to a large extent
influence its effectiveness for making quality product as well as the length of service it
will give. In making any changes to the operation, the welfare of the catalyst must be
given prime consideration for it can be regarded as the heart of the operation on which
the quality of the results obtained will depend.
In the discussion, which follows, the "product isomer ratio" refers to the weight
percentage ratio of isopentane to total C5 aliphatic paraffins, or the weight percentage
ratio of 2,2 and 2,3 dimethyl butane to the total C6 aliphatic paraffins in the stabilizer
bottoms stream. This is also expressed in the PIN-number as is shown in Figure 3.3.1.
The term "liquid feed", "reactor charge" and "combined feed", refers to the C5/C6 charge
to the liquid feed driers of the unit, the effluent from the liquid feed driers and the reactor
charge plus make-up hydrogen respectively.
Table 3.1- Properties useful in predicting isomerate product quality
Sp. Gr. RVP Molecular Octane Octane Octane Octane

Component 60F/60F psi Weight RON-O RON+3 MON-O MON+3
Isobutane 0.5631 71.90 58.120 100.2 106.7 97.6 120.0
n-Butane 0.5844 51.50 58.120 95.0 105.0 93.5 106.0
Isopentane 0.6248 18.93 72.146 93.5 104.5 89.5 106.9

n-Pentane 0.6312 14.42 72.146 61.7 84.7 61.3 83.8
Cyclopentane 0.7505 9.18 70.130 102.3 111.1 85.0 95.2
2,2 Dimethylbutane 0.6540 9.13 86.172 94.0 104.5 95.5 114.5

2,3 Dimethylbutane 0.6664 6.85 86.172 105.0 112.0 104.3 110.0
2 Methylpentane 0.6579 6.27 86.172 74.4 92.2 74.9 92.4
3 Methylpentane 0.6690 5.56 86.172 75.5 92.3 76.0 92.6
n-Hexane 0.6640 4.59 86.172 31.0 65.3 30.0 63.5
Methylcyclopentane 0.7535 4.17 84.156 96.0 104.5 85.0 91.1

Cyclohexane 0.7834 3.02 84.156 84.0 97.4 77.2 87.3
Benzene 0.8846 2.98 78.108 120.0 120.0 114.8 114.8
C7+ (Feed) 0.6915 1.97 100.198 55.0 78.0 55.0 79.0

C7+ (Product) 0.6830 2.10 100.198 82.0 88.0 71.0 88.0
Notes:
1. Octane values should be calculated based on liquid volume percent blending.
2. RVP values should be calculated based on mole percent blending.
3. RON-0 : Research Octane Number ASTM D2699.
MON-0 : Motor Octane Number ASTM D2700
RON+3 : Research Octane Number ASTM D2699, under the addition of
3.0 cc/gal tetraethyllead (TEL).
MON+3 : Motor Octane Number ASTM D2700, under the addition of
3.0 cc/gal TEL.
3.1.1 REACTOR TEMPERATURE

In general, reactor temperature is the main process control. A definite upper limit exists
for the amount of iso-paraffins which can exist in the reactor product at any given outlet
temperature, as shown in Figures 3.3.2, 3.3.3 and 3.3.4. This is the equilibrium imposed
by thermodynamics and it can be reached only after an infinite length of time, i.e. with an
infinitely large reactor. In practice, therefore, the product will contain less than this
equilibrium concentration of isoparaffins. As reactor temperature is raised to increase the
rate of isomerization, the equilibrium composition will be approached more closely. At
excessively high temperatures, the concentration of iso-paraffins in the product will
actually decrease because of the downward shift in the equilibrium curve, even though
the high temperature gives a higher reaction rate.
The equilibrium curves provided in Figures 3.3.2, 3.3.3 and 3.3.4 show vapor and liquid
phase equilibrium. At the process conditions in the H.O.T. Penex reactor the composition
is mixed phase. The amount of liquid is determined by the feed composition, reactor
temperature and pressure. The equilibrium values for liquid phase operation are lower
than for vapor phase operation. The actual equilibrium values for isopentane and 2,2
DMB for the mixed phase content of the reactor lies between the liquid and vapor curves
shown in Figures 3.3.2, 3.3.3 and 3.3.4.
The use of temperatures higher than necessary to achieve a reasonably close approach
to equilibrium accomplishes nothing other than to increase the amount of hydrocracking.
Extremely high temperatures may lead to an increased rate of carbon laydown on the
catalyst; however, the carbon forming propensity of the catalyst is inherently so low that
excessive hydrocracking would normally be encountered before carbon formation
problems would develop. It is recommended, however, that UOP be consulted before
temperatures above about 204°C at reactor outlet are employed.
This C5/C6 isomerization unit has two series reactors with provision for independent
temperature control. The first reactor system effects the bulk of the isomerization, so long
as most of the catalyst therein is still active. Any benzene in the feed is hydrogenated in
the first reactor, even when the catalyst therein has lost its activity with respect to paraffin
isomerization. Some conversion, ring opening, of cyclohexane and methyl cyclopentane
to hexanes also occurs, as does some hydrocracking of C7 to C3 and C4. These three
reactions (benzene hydrogenation, naphthene ring opening to hexane, and C7
hydrocracking) are exothermic and, for a typical feedstock contribute more to the
temperature rise in the first reactor than does paraffin isomerization, which is also
exothermic.
Normally, the first reactor system will be operated at such a temperature as to maximize
the concentration of isopentane and 2,2 dimethyl butane in its effluent. The
concentrations attainable and the required outlet temperature will be influenced by the
amount of active catalyst present and by the amount of C6 cyclic and C7+ components
present in the feed, higher the temperatures being required with high concentrations of
these components in the feed. By this procedure, the required operating temperature on
the second reactor system is reduced and it is possible to operate under conditions
where the equilibrium is more favorable.
Although the first reactor system temperature is normally selected without regard to the
isomer content of the final stabilizer bottoms product, there are the possible interactions
which should be considered for optimum overall operation, the quantitative relationships
for which will be developed through operating experience on each unit and which will
vary with catalyst age. Provided the final product can be made as rich in isopentane and
2,2 dimethyl butane (after optimization of the second reactor temperature) then the first
reactor is better operated with a lower iso-pentane and 2,2 dimethyl butane content in its
effluent, because this implies a lower first-reactor temperature and, therefore, slightly
less hydrocracking and slightly higher liquid yield. This situation is more likely to arise in
the early stages of a run when all of the catalyst is fresh. The second interaction may
occur with feeds, which are rich in C6 cyclics. Since these materials tend to reduce the
rate of paraffin isomerization, it may be beneficial with very C6 cyclic rich feedstocks to
choose the first reactor temperature to control the amount of cyclics, which enter the
second reactor. By raising the first reactor temperature, more of the cyclics can be
converted to hexanes and the rate of isomerization in the second reactor system thereby
increased.
The best combination of reactor temperatures for each plant will be easily determined
through operating experience. See also Figure 3.3.5.
Table 3.2 - Naphtha fractionation
Component Boiling Point (C) Relative Volatility

Isopentane 28 3.18
n-Pentane 36 2.71
2,2 Dimethylbutane 50 1.90
2,3 Dimethylbutane 58 1.59
2 Methylpentane 60 1.53
3 Methylpentane 63 1.42
n-Hexane 69 1.26
Methylcyclopentane 72 1.21
Benzene 80 1.25
Cyclohexane 81 1.00
3.1.2 LIQUID HOURLY SPACE VELOCITY

This term, commonly shortened to LHSV, is defined as the volumetric hourly flow of
reactor charge divided by the volume of catalyst contained in the reactors in consistent
units. The design LHSV for C5/C6 Penex operation is normally between 1 and 2.
Increasing the LHSV beyond this will lead to lower product isomer ratios.
In order to avoid excessive reactor severity, the H.O.T. Penex reactor LHSV should
always be maintained above 0.5 Hr.-' overall or 0.1 LHSV minimum per reactor.
3.1.3 HYDROGEN TO HYDROCARBON MOL RATIO

This ratio is defined as the number of mols hydrogen at the reactor outlet per mol of
reactor charge passing over the catalyst, and is specified at 0.05 mols H2/mol HCBN.
The primary purpose of maintaining the ratio at or above the design is to avoid carbon
deposition on the catalyst and maintain enough H2 for the reactions to proceed. If
necessary, the reactor charge rate is to be reduced to maintain the design hydrogen to
hydrocarbon ratio. The H2/HCBN ratio is determined by measuring the total mols of
hydrogen in the Stabilizer Overhead Gas (023-AT-003) and dividing by the total moles of
fresh Feedstock (023-FIC-009).
3.1.4 PRESSURE
This Penex unit is designed to operate at 31.7 kg/cm² g at the reactor outlet.
Methylcyclopentane and cyclohexane appear to adsorb on the catalyst and reduce the
rate of isomerization reactions. Higher pressure helps to offset this effect of the C6 cyclic
compounds. Lowering the unit pressure or operating at a slightly lower level would not
affect the catalyst life but the extent of isomerization would be influenced.
3.1.5 CATALYST PROMOTER

To sustain catalyst activity, the addition of chloride is necessary. At no time should the
plant be operated for longer than six hours without the injection of chloride. Whenever
there is a catalyst chloride deficiency, the product isomer ratios will decrease (although
not necessarily instantaneously), other things being equal. Restarting the injection of
chloride will tend to return the activity of the catalyst to its previous level, but it is possible
that full activity will not be restored if a decline in activity as a result no chloride injection
has been observed. Isomerization grade perchloroethylene (C2Cl4) is UOP's
recommended source of chloride.
Table 3.3 - Properties of Perchloroethylene
Perchloroethylene
Formula C2CI4
Molecular weight 165.8
Boiling point 121 °C
Melting point -23°C
Specific gravity (20/20°C) 1.62
Chloride content, wt% 85.5
3.1.6 PROCESS CONTAMINANTS

General
The purpose of this section is to discuss and highlight the effects of the following
contaminants and undesirable components on the Penex Process.
Contaminants
1. Sulfur
2. Water or other Oxygenated Compounds
3. Nitrogen
4. Fluoride
Undesirable Hydrocarbons
1. Olefins
2. Cyclic Compounds
3. C7 Hydrocarbons
4. Butane
As the Penex unit's feed is hydrotreated and dried, it is highly unlikely that any of these
contaminants will manifest themselves to any degree.
Table 3.4 - Typical limits on stream impurities
Impurity Typical Limit Laboratory Method

Penex Reactor Charge
Total sulfur ppmw 0.1 UOP-727
Total nitrogen ppmw 0.1 UOP-384
Total oxygenates ppmw 0.1 *
Water ppmw 0.05 On-Line Analyzer
Copper ppbw Nil UOP-144
Lead ppbw Nil UOP-350
Arsenic ppbw Nil UOP-296/UOP-387
Fluorides ppmw 0.5 UOP-619
Bromine number 4 ASTM-1159
Total chloride ppmw 0.5 UOP-395
Penex Make-up Gas
Hydrogen sulfide mole-ppm 1 Draeger Tube
Total nitrogen ppmw 1 UOP-430
Water ppmv 0.1 On-Line Analyzer
HCl mole-ppm 5 Draeger Tube
Total carbon oxides mole-ppm 10 UOP-603
CO mole-ppm 1 UOP-603
* Present method dependent on type of oxygenate.

However, as it is possible for unit upsets and misoperation, their detrimental impact on
the process is presented.
3.1.6.1 Contaminants
1. Sulfur
The presence of sulfur in the combined feed will decrease the activity of the catalyst.
This decrease in activity is temporary and recovery is normally rapid once the sulfur
has been removed. An increase in reactor temperatures to purge sulfur from the
catalyst more rapidly may be desirable after the sulfur has been removed from the
combined feed. While sulfur is present in the feed, an increase in temperature may
help to partially compensate for the reduced catalyst activity. A sulfur stripping
operation will be necessary if performance is unacceptable after elevating reactor
temperatures.
2. Water or other Oxygenated Compounds
The deactivation resulting from these compounds is permanent. Approximately 1 kg
of oxygen in any form will deactivate 100 kg of catalyst. The oxygenated compounds
react chemically with the active chloride on the catalyst. This chloride is chemically
bound into the alumina structure during manufacture. The water, once it reacts with
the catalyst and thereby splits out HCl, is chemically bound as hydroxyl to the
alumina.
3. Nitrogen Compounds
These compounds normally react with the chloride in the catalyst or the HCl to form
salts, which can deactivate the catalyst permanently by coating the catalyst active
sites, loss of chloride or maldistribution due to salt deposits.
4. Fluoride Compounds
This material is also a permanent catalyst poison. Approximately 1 kg of this material
will deactivate 100 kg of catalyst.
Although the Penex Process will tolerate certain hydrocarbon components, they
should be minimized in the feedstock to assure optimum unit performance.
3.1.6.2 Undesirable Hydrocarbons

1. Olefins
The UOP Penex Process has been operated with an olefin content of as much as 2%.
The amount and types of olefins present in, say, a C5/C6 fraction from a catalytic
reformate are acceptable, but highly olefinic streams of thermal or FCC origin cannot
be handled without prior hydrogenation to saturate the compounds. The adverse
effect of appreciable quantities of olefins is thought to be due to their physically
coating the catalyst following polymerization.
2. Cyclic Compounds
Although this is not a cumulative effect at normal operating pressures, cyclic
compounds are absorbed on the catalyst and therefore reduce the active sites
available for paraffin isomerization. (Should the amount of benzene in the charge
stock exceed about 5%, additional catalyst inventory would be required in the
reactors.)
Unsaturated cyclic hydrocarbons consume considerable quantities of hydrogen,
resulting in an exothermic reaction, which is undesirable from the standpoint of
isomerization equilibrium. Benzene is quickly hydrogenated and then behaves as an
equivalent amount of cyclohexane. Cyclohexane and other C6 naphthenes are
converted to C6 paraffins. This results in a decrease in octane number for this portion
of the charge stock. With normal fractionation, however, any attempt to eliminate C6
cyclics will result also in an exclusion in part of the normal hexane. Special
fractionation facilities are not required for the UOP Penex Process (see Figure 3.3.6
and 3.3.7).
3. C7 Hydrocarbons
It is preferable to restrict the C7+ content of the feedstock to the UOP Penex Process
using I-8 Plus and I-82 catalysts to 2 or 3%. C7 paraffins hydrocrack quite readily to
C3 and C4, and those, which do not hydrocrack will be isomerized to a mixture having
a lower octane number than the C5 or C6 produce and will thus degrade the overall
product octane number. C7 naphthenes have the same adverse effect as the C6
naphthenes described above, but to an even greater degree. Of course, the levels of
the cyclic and C7 hydrocarbons above mentioned are not normally expected unless
there are plant upsets on the prefractionation equipment proceeding the unit (see
Figure 3.3.6 and 3.3.7).
4. Butane
There is no particular concern as to the actual limits as far as harm, which could
occur to the reaction process with the inclusion of butanes in the feedstock. Normally,
4 LV-% is acceptable.
Figure 3.3.1
Figure 3.3.2
Figure 3 . 3 . 3
Figure 3 . 3 . 4
Figure 3 . 3 . 5
Figure 3 . 3 . 6
Figure 3 . 3 . 7
3.2 PROCESS VARIABLES OF DIH

The purpose of this section is to discuss the principal process variables and examine the
effect these have on DIH performance. The process variables, which will affect the
column, are:
Feed Composition
Pressure
Inlet Temperature
Reflux/Feed Ratio
Reboiler Heat Input
Side Draw Recycle Rate
Side Draw Tray Temperature
3.2.1 FEED COMPOSITION
DIH performance is related to the type of feed that is charged to the column. If the
feed is different from design specifications, then the DIH may not be able to make the
desired separation. Since feed composition is not a variable that is easily
manipulated, it is usually good practice to check the feed being sent to the DIH on a
daily basis (SCC-2304). Feed that is significantly different than design (more heavies
or light ends) will upset the DIH operation and produce off-spec product.
A change to a lighter feed will tend to require a lower top tray temperature to maintain
the same recovery of pentanes and 2,2 DMB material in the net overhead. A heavier
feed will tend to require the opposite.
The extent of the DIH sensitivity to feed composition swings also depends on how
conservatively the column has been designed. If there is enough capacity in the
Reboiler to accommodate more duty and the column has extra trays, then operation
can be customized to specific changes in feed composition. Normally a 10-20%
change in composition does not affect performance significantly.
3.2.2 PRESSURE
The DIH pressure is a variable that is typically fixed by design and is not adjusted.
Adjusting the pressure will change the vapor loads and could cause the column to
flood if the pressure is changed significantly. The change in the vaporization rate in
the column is inversely proportional to the change in the absolute pressure in the
column. DIH columns are designed to operate in a very limited pressure range. A DIH
runs anywhere from 0.3-1.0 barg.
Only small changes can be made to column pressure. For example, a reduction from
15 psig to 10 psig will increase the vaporization rate by (15+14.7)/(10+14.7)=1.20
times or an 8% increase. This change could flood the column and cause the separation
efficiency to fall dramatically.
Generally, a move in pressure is used to "fine tune" a column rather than change
composition significantly as part of an advance control scheme. Lower operating
pressures in general increases the relative volatility of the component, which
increases the efficiency of the separation. This in turn decreases the reflux requirement
for a given number of trays resulting in a decrease in reboiler duty.
Regardless, good column operation requires that pressure be held stable. Continuous
changes will upset the column and do more harm than good.
3.2.3 INLET TEMPERATURE

The DIH feed temperature is heat integrated with the side draw stream of the DIH
column by the DIH side draw reboiler E-2312.
During column design, the feed inlet is chosen to be at that point in a column where
feed, tray composition and temperature are the same. A sudden change to a colder
feed will act as reflux and will push the reboiler harder to maintain the liquid at its
bubble point. This will upset the DIH heat balance and reduce column efficiency. It will
also upset the bottom net stream since more light ends will be sent through until
reboiler heat input is increased and column heat balance is re-established. The
overhead product will maintain purity but at a lower net flow since cooler material
(hence less light traffic at top of DIH) was sent up.
Too high an inlet temperature is similar to having the reboiler at a high duty and will
cause more heavy material to migrate into the overhead product. Compositional
temperature control will combat this by reducing product draw and increasing reflux to
obtain desired temperature and composition profiles.
3.2.4 REFLUX/FEED RATIO
This variable is dependent both on reboilers heat duty and top temperature control.
Separation efficiency will increase with reflux to feed ratio until the tower begins to
flood. This ratio is a good monitoring tool for an operator and can easily be displayed
on a DCS system.
Liquid reflux adjusts the top column temperature by taking out heat from the tower
through liquid vaporization. The higher the reflux, the cooler the temperature will be at
the top of the column.
The temperature required for the desired overhead product composition will depend
on tower pressure and feed composition. As already discussed, if the DIH pressure
goes down, the temperature controller will also have to be adjusted down to maintain
the same overhead feed composition. If the feed composition gets lighter, then the
composition in the overhead will be lighter.
3.2.5 REBOILERS HEAT INPUT
The heat input to the column is provided by the DIH reboiler E-2316 and the side
draw reboiler E-2312. The side draw reboiler heat input is calculated through a heat
input calculator XY-005. There is no direct control on this variable.
The column reboiler (E-2316) flow rate is an independent variable that controls the
heat input into the DIH.
When additional heat is put into the tower, it will be removed with additional reflux and
possibly net overhead product to maintain the tower energy balance. For a given feed
rate and tower top temperature, the reboilers heat input will directly adjust the reflux to
feed ratio. A higher reflux rate will improve the separation until the tower begins to
flood. When the column floods, tray efficiency drops due to entrainment of liquid up
the column. The higher efficiency at a higher reflux is an additional cost in the form of
higher utilities consumption.
In general, reboilers heat input should be adjusted to the given minimum reflux
required to make the separation for a given feedstock. At less than 50% of design
flow, the reflux/feed ratio and therefore reboilers heat/feed ratio will have to be
increased due to a drop off in the tray efficiency at the turndown condition.
3.2.6 SIDE DRAW RATE
The DIH recycle side draw is taken off as a lower side cut. The side cut is pumped
back to the isomerization unit upstream of the liquid feed driers DR-2303/2304. The
FIC on the side draw (023-FIC-030) can be cascaded from the draw tray temperature,
but is in this column cascaded from the column bottoms LIC (023-LIC-014).
The bottoms flow to storage is on flow control (023-FIC-028). This is typically such a
small flow that cascading it from the bottoms LIC (023-LIC-014) would cause upsets
to the column.
3.2.7 SIDE DRAW TRAY TEMPERATURE
The side draw temperature is typically set based on the composition of the side draw
recycle back to the isomerization unit. The heavies on the side cut should be
minimized to obtain the best performance from the isomerization reactor section. The
side draw tray temperature should also be optimized to obtain maximum
methylpentanes in the side cut, while maximizing 2,3 DMB in the overhead product.
Side draw tray temperature will depend directly on side draw reboiler heat input. If
side draw reboiler heat input is too high, side draw tray temperature will increase and
cause more heavy material to migrate into the overhead product.
If side draw reboiler heat input is too low, side draw tray temperature will decrease
and light isomerate will flow through side draw. In this case, 023-AIC-004 A/B will be
off spec and will cause net overhead product flow rate to be increased, which will
entail reflux flowrate to decrease to obtain desired temperature and composition
profiles.

Signals exchanged with other units:
Equipment TAG N°
Origin D-1208 (Makeup Gas Knockout 012-LXAHH-017
Drum/Lube Oil Mist Eliminator)
(PID 012-PID-0021-025)
Destination A-2302 (Methanator Heater) 023-UX-013 (Methanator Heater
(PID 023-PID-0021-010) shutdown
A high high liquid level in the Makeup Gas Knockout Drum / Lube Oil Mist Eliminator D-
1208 shall cause Methanator Heater shutdown.

Text to be prepared by JVD Electricity and Instrument Managers.

N/A
CHAPTER 4
UTILITY, CHEMICAL AND CATALYST REQUIREMENTS
CONTENTS
1. UTILITIES
1.1 UTILITIES CONSUMPTION SUMMARY
1.2 ELECTRICAL LOAD SUMMARY
2. CHEMICAL CONSUMPTION
2.1 CATALYST AND CHEMICAL SUMMARY
2.2 CHEMICAL HANDLING
2.2.1 CAUSTIC INJECTION
2.2.2 CHLORIDE INJECTION PACKAGE X-2302
2.2.3 ISOMERIZATION CATALYSTS LOADING

1. UTILITIES
1.1 UTILITIES CONSUMPTION SUMMARY

For Fuel Gas, Steam, Electrical Power, Cooling Water, Water, Nitrogen and Plant and
Instrument Air consumptions, refer to following documents:
8474L-023-CN-0003-001 Estimated Utility Consumption - DESIGN CASE -

100% Bach Ho or Mixed crude, Max Gasoline or
Distillate
8474L-023-CN-0003-002 Estimated Utility Consumption - NORMAL CASE -
100% Bach Ho, Max Gasoline or Distillate
8474L-023-CN-0003-003 Estimated Utility Consumption - NORMAL CASE –
Mixed crude, Max Gasoline or Distillate
1.2 ELECTRICAL LOAD SUMMARY
The electrical load of each equipment of the Isomerization Unit is given in the hereafter
document:
8474L-200-CN-1626-001 Electrical Load Summary

2. CHEMICAL CONSUMPTION
2.1 CATALYST AND CHEMICAL SUMMARY
Isomerization catalysts are I-8 Plus Penex Catalyst and I-82 Penex Catalyst from UOP.
Catalysts used in Methanator are Sulfur absorbent Puraspec 2443 and Methanation
catalyst Puraspec 2010 from Johnson Matthey.
Molecular sieves required for Makeup Gas Driers are Molsiv Adsorbent type PDG-418
from UOP.
Molecular sieves required for Feed Driers are Molsiv Adsorbent type HPG-250 from
UOP.
Caustic used for injection in Net Gas Scrubber is 14.4wt% caustic from Caustic Supply
Unit 039.
Chloride used is Perchloroethylene.
The catalyst and chemical summary of the Isomerization Unit is given in the hereafter
document:
8474L-023-CN-0004-502 PENEX Catalyst and Chemical Summary
The properties of the chemicals and catalysts are given in the Material Safety
Datasheets in attachment.
2.2 CHEMICAL HANDLING
2.2.1 CAUSTIC INJECTION

Caustic for injection in net gas scrubber is provided from Caustic Supply Unit 039 (14.4wt%
caustic) by mean of either of 20°Be Caustic Transfer Pumps (P-3903 A or B) and diluted to
10wt% with water. It is then routed to Net Gas Scrubber T-2302 by mean of Caustic Transfer
Pump P-2306.
2.2.2 CHLORIDE INJECTION PACKAGE X-2302

Chloride Injection Drum (D-2302) is fed in perchloroethylene by mean of Chloride Transfer
Pump P-2302. Chloride is supplied with chloride drums of 200L each. A rack for 10 drums
and means for placing drums on rack are provided. Quick connects with double end shut-off
are provided for each drum.
2.2.3 ISOMERIZATION CATALYSTS LOADING

The I-8 Plus and I-82 Penex catalysts are shipped in sealed 55-US gallon drums that a
special protective lining. Special care should be taken as any rough handling could cause
the protective lining heat seals to be broken. Catalysts are dense loaded. Before, during and
after catalysts loading, special care should be taken to protect catalysts from moisture at all
times as any contact with water or air will result in permanent deactivation of the catalysts.
CHAPTER 5
PREPARATION FOR INITIAL START-UP
CONTENTS
1. PLANT CHECK-OUT
2. LINE FLUSHING
4. LEAK TESTING (AT 8 KG/CM² G)
5. HEATER DRY-OUT
6.1 INTRODUCTION
6.2 CATALYST / ADSORBENT / MOLECULAR SIEVE STORAGE
6.3 DRUM HANDLING
6.4 PRE-CHARGING CHECKS
6.5 LIST OF EQUIPMENT AND TOOLS NEEDED FOR CATALYST / ABSORBENT / MOLECULAR
SIEVE LOADING
6.6 METHANATOR LOADING
6.7 DRIERS
6.7.1 LIQUID FEED DRIERS
6.7.2 MAKE-UP GAS DRIERS
6.8 NET GAS SCRUBBER
6.9 ISOMERIZATION REACTORS CATALYST LOADING
1. PLANT CHECK-OUT
This chapter deals with precommissioning operations that will be described in PP-903.
2. LINE FLUSHING
4. LEAK TESTING (AT 8 KG/CM² G)

5. HEATER DRY-OUT
6.1 INTRODUCTION
The efficient and successful operation of the PENEX unit depends on the condition of the
purification materials (absorbent/adsorbent) and catalysts employed. The proper care of
catalyst does not always receive the attention that it deserves, even though the economic
success of the plant is closely linked to the way the catalysts are handled and treated in
service. Catalyst handling should be done with due care. In addition since many catalyst
handling operations have the potential for creating dusty working atmospheres, care must
be taken to adopt procedures which minimize the creation of dust. Suitable protective
clothing should be worn at all times when catalysts are being handled. In addition goggles,
gloves and dust masks are essential.
6.2 CATALYST / ADSORBENT / MOLECULAR SIEVE STORAGE

The I-8 Plus/I-82 Isomerization catalysts are shipped in sealed 55-US gallon drums that
have a special protective lining. The catalysts are contained in a heavy plastic bag with a
long neck. The neck is crimped in two places with wire and heat-sealed at the end. This bag
is inside another heat-sealed plastic bag (see Figure 6.2.1).
NOTE: ANY CONTACT WITH WATER OR AIR WILL RESULT IN PERMANENT DE-
ACTIVATION OF CATALYST.
Sulfur adsorbent and molecular sieve desiccant are shipped in mild steel drums with
polythene liners.
The drums should be inspected carefully when they arrive on site for damage in transit, so
that any insurance claim can be properly supported.
Drums must not be stacked on their sides or stacked more than four drums high, even when
held on pallets. Taller stacks tend to be unstable and the lower drums can be crushed.
Metal drums are usually suitable for outside storage for a few months, but should be
protected against rain and standing water. If prolonged storage is expected or if the drums
are not of metal, they should be kept under cover and away from damp walls and floors.
The lids should be left on the drums until just before the catalyst is to be charged, and if the
lids are accidentally knocked off or removed for inspection, it is important that they should
be replaced as soon as possible, so that contamination of the catalyst is avoided.
If the drum lid cannot be replaced, then the catalyst should be re-drummed without delay. If
any contamination occurs it is difficult to assess the extent of damage, and an analysis of a
sample may not give an adequate indication because of the difficulty of getting a typical
sample. If there is any doubt about the state of the catalyst, it is best not to charge it to the
equipment concerned.
6.3 DRUM HANDLING

Drums should be handled as gently as possible. Suitable space is required for storing the
drums between delivery and charging, and double handling can be avoided if this space is
close to the equipment to be loaded.
If a mobile crane or forklift truck is to be used for drum handling, a smooth paved area is
desirable to facilitate movement.
When drums are to be lifted to the charging manhole it is generally most satisfactory to use
a mobile crane rather than the individual lifting beam on the vessel, because a crane can lift
drums off a wide area and this avoids multiple handling.
Drums must not be rolled and, if manhandling is unavoidable, suitable drum barrows,
upending levers and skids should be provided. Special care should be taken with the I-8
Plus/I-82 Isomerization catalysts drums, as any rough handling could cause the protective
lining heat seals to be broken.
NOTE: ANY CONTACT WITH WATER OR AIR WILL RESULT IN PERMANENT DE-
ACTIVATION OF THE I-8 PLUS/I-82 CATALYSTS.
Drums are generally supplied on pallets, which reduces the likelihood of damage in transit,
but requires a suitable forklift for unloading at site storage.
The forklift truck to be used for dismantling the pallets should be fitted with rim or body
clamps to avoid damage to the drums.
6.4 PRE-CHARGING CHECKS

The methanator, make-up gas and liquid feed driers will be loaded in the same way, via the
top manhole.
After the manhole cover is removed (hand holes closed), inspect the interior of each vessel;
that to ensure that the vessel is clean, dry and free from loose scale and debris. It is not
necessary for the vessels to be bone dry, but any free water should be removed.
Inspect the grid supports and screens to ensure that the screens are properly overlapped
and that the edges of the screen are properly sealed and firmly held down (no gaps, no
holes). Faults at this point are difficult, if not impossible, to rectify once the catalyst is in
place.
It is important to ensure that the charging level is clearly defined, so as to avoid under- or
overfilling. All measurements should be made from a fixed reference point at the top of the
vessel. Guidance marks should be made on the vessel internal by means of black board
chalk, showing levels of the different size ceramic balls, sulfur absorbent, methanation
catalyst and molecular sieve desiccant bed height and top layers of ceramic balls.
An inventory of sulfur absorbent, methanation catalyst, molecular sieve desiccant and
ceramic support should be made well in advance, to ensure that sufficient quantities have
been supplied.
When the loading procedure is scheduled as a round-the-clock operation, adequate lighting
should be provided for safe nighttime activity in the work area.
The location of drums in the unit area and the stacking of empty drums should be planned in
advance to prevent confusion while vessel loading is underway. The drums should be
brought to the vicinity of the vessel as they are needed so that drums are not left in the open
should a hold-up in the loading procedure occur. The numbers of the drums should be
noted and checked against the list of drum numbers supplied by the manufacturer. Even if
these numbers have been checked on delivery the process should be repeated immediately
before the catalyst is loaded and record taken of the drum numbers in the sequence of
loading. Any drums with anomalous or ambiguous numbering should not be loaded but set
on one side and checked with the manufacturer.
The catalyst should be loaded to the specified bed height and the depth and weight of
catalyst loaded must be recorded. The weight of catalyst material rejected during screening
must be recorded and allowed for.
The drums should not be unsealed until just prior to loading. The lids should be removed at
such a rate, say four at a time, such that no catalyst is exposed to the air for longer than
necessary. This makes it simpler to protect the catalyst with the onset of bad weather. The
catalyst must be kept dry and unless effective covering can be provided, loading must be
discontinued when there is danger of the catalyst getting wet.
The catalyst should be handled as gently as possible. Multiple handling of drums should be
minimized and a drum should never be rolled; suitable equipment should be provided to
make this possible.
It is inevitable that from time to time some attrition will occur during catalyst transportation
and it may be necessary to screen before charging. Great care must be taken with this
operation since it is possible to degrade the catalyst pellets, beads. During the screening
operation the quantity of dust being collected should be checked. It should be less than 1 %
wt. If this is exceeded the entire operation should be suspended and reviewed.
The weight of the fines should be recorded and deducted from the weight of catalyst
discharged from the drums onto the screen. Care must be taken not to overload the screen
or inefficient screening will result.
When the drums have been opened the catalyst should be visually inspected. Any doubtful
material should be rejected until further inspection is possible.
Fresh catalyst should be sampled. A convenient way of doing this is to take a sample after
the catalyst leaves the screen or drum. One sample should be taken from each drum in
such a manner that material representative of the central half of the drum is obtained, not
material from the ends. These samples should subsequently be combined by coning and
quartering to provide one sample of 1 kg weight representing each 500 mm depth of catalyst
in the catalyst bed. The upper and lower levels represented by each batch of samples
should be recorded after leveling the catalyst bed and measuring the depth from a known
reference mark. Another method, which may be preferable when a man is to be inside the
vessel during charging, is to take representative samples from the bed surface after it has
been leveled at 300 mm intervals. Five samples should be taken at each level, one from the
center and 90° apart. These individual samples should subsequently be combined by
coning and quartering to give a 1 kg representative sample of the catalyst at that level. All
samples should be labeled in such a way that the label cannot become detached nor the
information erased.
The information should include:
♦ Plant, stream and vessel.
♦ Date of sampling.
♦ Numbers of drums represented by the sample.
♦ Position of the contents of the drums in the catalyst bed-upper and lower limits.
♦ Since entry into the vessel is required to properly load and level catalyst, the vessel must
be prepared for safe entry.
Install blind flanges on all in and outlet piping to prevent accidental release of
hazardous fluids into the vessel. Before each entry, have safety personnel analyze
the atmosphere in the vessel to make sure it is safe to breathe.
Use atmospheric air to vent the vessel. Never use plant air supply to provide air for
ventilation. The air supplied might be contaminated, or the supply could, by mistake,
be piped to a gas other than air.
Only a properly trained and equipped worker should enter the vessel. A safety harness and
rope should always be attached to that worker. Two properly trained and equipped co-
workers standing outside the entry port should constantly observe the worker in the vessel.
The co-workers should use the safety rope to prevent falls from the ladder used to enter or
leave the vessel. Also, if disabled, the worker can be removed using the rope.
Before any catalyst is loaded, it must be first decided how the catalyst is to be lifted to the top
of the reactor. It could be lifted in its original drums by a pulley system. But the quickest and
probably the best way is to lift the catalyst by a crane if one is available. If a crane is used,
the loading time can be greatly reduced by constructing two large transfer hoppers to move
the catalyst from ground level to the top of the reactors. In this case, a transfer hopper
loading platform must be constructed in a convenient place close to the reactors. The
loading platform can be constructed of scaffolding and wooden planks or of any other
convenient material. The platform area should be at least large enough to accommodate
enough drums to load one hopper and to allow working room for the personnel who will do
the loading.
Regardless of the way the catalyst will be lifted, a temporary storage place near the reactor
must be found for the catalyst. The catalyst should be stored on pallets and completely
covered by canvas to give a certain measure of protection against the elements. A forklift or
some other means of moving the catalyst from this site to the loading platform (or to any
other place), should be available.
The catalyst loading path, both on the ground and through the air, must be checked so that
it is entirely free from obstruction.
6.5 LIST OF EQUIPMENT AND TOOLS NEEDED FOR CATALYST / ABSORBENT /

MOLECULAR SIEVE LOADING
♦ Mobile crane.
♦ Forklift.
♦ Two large transport hoppers and separate lifting cables for each hopper.
♦ One transfer hopper loading platform if transfer hoppers are used.
♦ One filling funnel to rest at the top manhole of the reactor (for methanator + driers).
♦ Explosion proof light for inside the reactor (24 V), plus flash lights (2*).
♦ Canvas for covering the catalyst drums and vessel inlets, for protection against ingress
of rain.
♦ A safe ladder (rope), for inspection of vessel internals, having sufficient length for all
vessels.
♦ Loading socks of correct diameter and sufficient length.
♦ Wooden boards to stand on while inside the vessel and for leveling the catalyst.
♦ Eventually a vacuum eductor to remove catalyst dust in reactors.
♦ Protection equipment for loaders, dust masks, gloves, goggles etc.
♦ Chalk, crayons or other type of markers, to mark the level of catalyst to be loaded.
♦ Miscellaneous hand tools, pliers, screwdrivers, spanners etc.
6.6 METHANATOR LOADING
When the methanator has been pressure tested, dried and cleaned it may be loaded.
The loading of the methanator will take place in two distinct stages. The first is the
installation of the catalyst support material before the unit is dried, the second is the
methanation catalyst and the sulphur absorbent loading, after the unit has finally been dried.
Since the methanation catalyst is normally in the oxidized state when it is shipped to the
refiner, it will be possible to use standard sock loading practices. The catalyst vendor’s
loading and unloading instructions as well as the MSDS sheet for the catalyst must be
obtained and followed. The procedures below are meant as a guide and should be altered
as needed to match the vendor instructions.
Prior to and during the loading of the sulphur absorbent, certain precautions should be taken
to ensure that the absorbent will perform optimally. The absorbent is shipped in drums,
which should not be opened until just prior to be loading. Exposure to excessive moisture
can alter the chemical properties of the absorbent and thus reduce its effectiveness. Dust
mask and gloves must be worn to avoid irritation when handling the absorbent.
The methanator should be dried before loading.
a. With the completion of the sand blasting and oil coating, the reactor is ready for the
installation of the catalyst support materials.
b. Install the slotted cap over the bottom outlet. Check to ensure there is a good fit in order
to avoid passage of ceramic support between the bottom of the basket and the outlet
nozzle.
c. The support plates should be installed in the unloading nozzles and a coil of 13 mm
diameter ceramic fiber rope laid over them.
d. Install the sleeves in the unloading nozzles and fill with 6 mm balls to 100 mm from the
top. Add 100 mm of 3 mm diameter balls.
e. For the loading of the ceramic support, the upper manhole should be used. The balls
lowered by rope and bucket.
f. With the bottom internals in place, load 19 mm diameter balls up to a height of 320 mm
above bottom tangent line. The top of this layer should be leveled.
g. A 100 mm of 6 mm diameter balls is loaded on top of the 19 mm diameter balls, taking
care not to disturb the 19 mm balls. The top of the 6 mm layer to be leveled.
h. A 100 mm layer of 3 mm diameter ceramic balls is loaded on top of the 6 mm balls,
taking care not to disturb the lower layer and making sure each layer remains leveled.
i. Install inlet distributor and head up the reactors.
j. Install a hopper with a canvas sock at the top of the reactor and adjust the sock length so
that the catalyst will fall no more than five feet.
k. The canvas sock must be grounded.
l. Dress in proper safety clothing and clear non-essential personnel from tie area.
m. Load the methanation catalyst into the reactor and adjust the length of the canvas sock
as needed. Record the lot number and drum number from each catalyst drum and the
total weight loaded. Load catalyst to the height indicated on the loading diagram (bed
height of 4.400 mm).
n. Level the catalyst bed and measure the distance from the catalyst to the top of the
reactor manway flange.
o. Connect a nitrogen hose to the bottom of the methanator and start a small purge of
nitrogen through the vessel. The nitrogen purge should be maintained throughout the
absorbent loading to minimize absorbent contact with air.
p. Pour the sulfur absorbent into the reactor taking care not to disturb the methanation
catalyst bed. Record the lot number and drum number from each absorbent drum and
the total weight loaded. Load absorbent to a bed height of 850 mm.
q. Level the absorbent bed and measure the distance from the absorbent to the top of the
reactor manway flange.
r. Load a 100 mm layer of 6 mm ceramic balls on top of the absorbent. Load a 100 mm
layer of 19 mm balls on top of the 6 mm balls.
s. Install the ceramic holddown material and level (per the methanator reactor loading
diagram).
t. The vessel may be headed up after checking that the inlet distributor is properly
installed. All rings and flanges should be thoroughly cleaned before assembly.
u. Close the reactor.
v. Remove the isolation blinds.
6.7 DRIERS
When the make-up gas/liquid feed driers have been pressure tested, dried and cleaned,
they may be loaded.
Prior to and during the loading of the molecular sieve desiccant, certain precautions should
be taken to ensure that the molecular sieve will perform optimally. The molecular sieve is
shipped in drums, which should not be opened until just prior to loading. Exposure to
excessive moisture should be avoided. Therefore, the driers must be kept free of water.
Molecular sieve is normally sock-loaded into the drier. Dust masks and gloves must be worn
to avoid irritation when handling the molecular sieve. The drier vessels should be dry before
molecular sieve is loaded. The hopper and loading sock used for loading are shown in
Figure 6.7.1.
a. Install the support cap over the bottom nozzle. Check to assure there is a good fit in
order to avoid passage of support material between the bottom of the support cap and
the bottom nozzle. 6 mm ceramic rope may be required as packing around base of
support cap.
b. For loading of the ceramic support and the molecular sieve, the upper manhole should
be used.
c. With the bottom support cap in place, load 19 mm diameter ceramic balls up to a height
of 150 mm above vessel bottom tangent line. The top of this layer should be leveled.
d. A 150 mm layer of 6 mm diameter ceramic balls is loaded on top of the 19 mm balls;
again taking care to avoid disturbing the layer below and making sure each layer is
leveled.
e. A 150 mm layer of 3 mm diameter ceramic balls is loaded on top of the 6 mm balls; again
taking care to avoid disturbing the layer below and making sure each layer is leveled.
f. Connect a nitrogen hose to the bottom of the drier and start a small purge of nitrogen
through the vessel. The nitrogen purge should be maintained throughout the loading to
minimize molecular sieve contact with air.
g. For loading of the molecular sieve, use a hopper with a sock attached. Static electricity
may build up during sieve loading. It will be necessary to lower a metal weight fastened
to a wire or chain that has been grounded. This will discharge the build up of static
electricity. Shorten the chain and sock together as the sieve bed rises. Load sieve to a
bed height of 2.600 mm and level off.
NOTE: Personnel entering driers to install 20 mesh screen and 19 mm ceramic balls,
should be fully experienced in the use of fresh air breathers/air sets.
h. Install 20 mesh screen, ensuring 150 mm overlap at joints.
i. Load 150 mm of 19 mm balls on top of screen.
j. The vessel may be heated up after checking outlet pipe. All rings and flanges should be
thoroughly cleaned before assembly.
The loading diagram for the Feed Driers is shown in Figure 6.7.2.

a. Install the support cap over the bottom nozzle. Check to assure there is a good fit in
order to avoid passage of support material between the bottom of the support cap and
the bottom nozzle. 6 mm ceramic rope may be required as packing around base of
support cap.
b. For loading of the ceramic support and the molecular sieve, the upper manhole should
be used.
c. With the bottom support cap in place, load 19 mm diameter ceramic balls up to a height
of 350 mm above vessel bottom tangent line. The top of this layer should be leveled.
d. A 150 mm layer of 6 mm diameter ceramic balls is loaded on top of the 19 mm balls;
again taking care to avoid disturbing the layer below and making sure each layer is
leveled.
e. A 150 mm layer of 3 mm diameter ceramic balls is loaded on top of the 6 mm balls; again
taking care to avoid disturbing the layer below and making sure each layer is leveled.
f. Connect a nitrogen hose to the bottom of the drier and start a small purge of nitrogen
through the vessel. The nitrogen purge should be maintained throughout the loading to
minimize molecular sieve contact with air.
g. For loading of the molecular sieve, use a hopper with a sock attached. Static electricity
may build up during sieve loading. It will be necessary to lower a metal weight fastened
to a wire or chain that has been grounded. This will discharge the build up of static
electricity. Shorten the chain and sock together as the sieve bed rises. Load sieve to a
bed height of 3.100 mm and level off.
NOTE: Personnel entering driers to install 20 mesh screen and 19 mm ceramic balls,
should be fully experienced in the use of fresh air breathers/air sets.
h. Install 20 mesh screen, ensuring 150 mm overlap at joints.
i. Load 150 mm of 19 mm balls on top of screen.
j. The vessel may be heated up after checking outlet pipe. All rings and flanges should be
thoroughly cleaned before assembly.
The loading diagram for the Make-up Gas Driers is shown in Figure 6.7.3.
6.8 NET GAS SCRUBBER

This net gas scrubber is to be carefully loaded with 19 mm Carbon Raschig rings. Care is to
be taken during loading since these rings are easily broken. Therefore, the tower is to be
filled with water to break the fall of the rings and once the rings are loaded, the hold-down
grating is to be installed. Then the water is to be drained and the loading manway closed.
Do not use berl or ceramic rings as they are attacked in a caustic environment.
NOTE: The opening, loading and closing of the reactors should be a continuous operation
with no breaks. During the opening, loading and closing of the reactors, a dry nitrogen
blanket MUST be maintained at all times
6.9 ISOMERIZATION REACTORS CATALYST LOADING

Refer to Chapter 6 §5.
Figure 6.2.1
Figure 6.7.1
Figure 6.7.2
Figure 6.7.3
CHAPTER 6
INITIAL AND NORMAL START-UP
CONTENTS

2.1 STEAMING
2.2 EVACUATING
2.3 NITROGEN PURGING

4.1 WATER WASH NET GAS SCRUBBER AND CHLORIDE INJECTION
4.2 REACTOR AND LINE SWITCHING
4.3 HYDROGEN ADDITION
4.4 HYDROCARBON ADDITION
4.5 REACTOR CIRCUIT CIRCULATION
6. CATALYST LOADING
6.1 LOADING VESSEL SUPPORT MATERIAL
6.2 I-8 PLUS / I-82 CATALYSTS LOADING
6.2.1 GENERAL
6.2.2 EQUIPMENT AND MATERIALS REQUIRED
6.2.3 CATALYST LOADING EQUIPMENT DETAILS
6.2.4 LOADING PROCEDURES
7. INITIAL START-UP
7.1 INITIAL OPERATION

7.2 SERIES FLOW OPERATION
8. NORMAL START-UP
8.1 START-UP AFTER TOTAL UNIT SHUTDOWN
8.2 START-UP AFTER PARTIAL CATALYST CHANGE-OUT OR SHUTDOWN
9. DE-ISOHEXANIZER START-UP

10.1 METHANATOR OPERATION
10.2 LIQUID FEED DRIERS OPERATION
10.2.1 BOTH DRIERS ON-LINE IN SERIES FLOW, WITH DRIER DR-2303 IN LEAD POSITION AND
DRIER DR-2304 IN LAG POSITION
10.2.2 BYPASS AND ISOLATE DRIER DR-2303 AND PLACE DRIER DR-2304 IN SINGLE DRIER
MODE
10.2.3 REGENERATE DRIER DR-2303
10.2.4 PLACE DRIER DR-2303 IN SERIES FLOW WITH DRIER DR-2304, WITH DRIER DR-2304 IN
LEAD POSITION
10.2.5 REPEAT SEQUENCE FOR DRIER DR-2304
10.3 MAKE UP GAS DRIERS OPERATION

10.3.1 BOTH DRIERS ON-LINE IN SERIES FLOW, WITH DRIER DR-2301 IN LEAD POSITION AND
DRIER DR-2302 IN LAG POSITION
10.3.2 BYPASS AND ISOLATE DRIER DR-2301 AND PLACE DRIER DR-2302 IN SINGLE DRIER
MODE
10.3.3 DEPRESSURE DRIER DR-2301 AND LIQUID FILL WITH REGENERANT
10.3.5 PLACE DRIER DR-2301 IN SERIES FLOW WITH DRIER DR-2302, WITH DRIER DR-2302 IN
LEAD POSITION AND DRIER DR-2301 IN LAG POSITION
10.3.6 REPEAT SEQUENCE FOR REGENERATION OF DRIER DR-2302
10.4 REACTOR OPERATIONS

10.4.1 PENEX REACTOR TEMPERATURES
10.4.2 LEAD REACTOR EFFLUENT SAMPLE
10.4.3 HYDROGEN TO HYDROCARBON RATIO
10.5 STABILIZER OPERATION

10.6 STABILIZER NET GAS SCRUBBER OPERATION
10.7 DE-ISOHEXANIZER COLUMN OPERATION

10.8 PREVENTIVE MAINTENANCE
10.9 TROUBLESHOOTING
10.10 TYPICAL EXAMPLE FOR COLLECTING DATA & QUALITY CONTROL
On the following page, a logic diagram is presented to summarize the different steps of
an initial start-up of the Isomerization Unit.
Start-up of Methanator system
Hydrocarbon circulation and initial drydown
Start water wash and chloride circulation

in Net Gas Scrubber
Reactor and line switching
Hydrogen addition
Hydrocarbon circulation
Reactor circuit circulation
Acidizing and final drydown
Isomerization reactors catalyst loading
Initial Start-up

It must be remembered that oil or flammable gas should never be charged into process lines
or vessels indiscriminately. The unit must be purged before admitting hydrocarbons. There
are many ways to purge the unit and ambient conditions may dictate the procedure to be
followed:
♦ Steaming followed by fuel gas blanketing.
♦ Evacuating the equipment followed by nitrogen blanketing.
♦ Nitrogen or inert gas purging.
2.1 STEAMING
Steaming followed by fuel gas blanketing is generally the most common technique used for
air freeing the fractionation section of the PENEX unit and de-isohexanizer. Thus, the
following steps will briefly outline this method:
a. Potential problems or hazards which could develop during the steam purge are as
follows:
Collapse due to vacuum
Some of the vessels are not designed for vacuum. These equipments must not be
allowed to stand blocked in with steam since the condensation of the steam will
develop a vacuum. Thus, the vessel must be vented during steaming and then
immediately followed up with an inert fuel gas purge at the conclusion of the steam-
out.
Flange and gasket leaks
Thermal expansion and stress during warm-up of equipment along with dirty flange
faces can cause small leaks at flanges and gasketed joints. These must be corrected
at this time.
Steam condensate hammering
Care must be taken to prevent condensate hammering when steam purging the unit.
Severe equipment damage can result from condensate hammering.
b. Block in the cooling water to all coolers and condensers. Shutdown fans on fin-fan
coolers and condensers.
c. Open high point vents and low point drains on the vessels to be steam purged.
d. Start introducing LP steam to the Stabilizer (T-2301) via 3”-SL-230518 and to the
Stabilizer Receiver (D-2303) via 2” Utility Connection, to the De-isohexanizer (T-2303)
via 3”-SL-230237 and to the De-isohexanizer Receiver (D-2306) via 2” Utility
Connection.
NOTE: In the de-isohexanizer section it may be necessary to make up additional steam
connections to properly purge some piping which may be "dead-headed".
e. Thoroughly purge all equipment and associated piping of air. The progress of the
steam purge can be followed by marking up a P&I diagram to indicate the lines purged.
Verify that sufficient drains are open to drain the condensate, which will collect in low
spots in the unit.
f. When the steam purging is completed, start to close all the vents and drains.
Immediately start to introduce fuel gas into all vessels and then cut back the steam flow
until it is stopped. Regulate the fuel gas flow and the reduction of steam, so that a
vacuum due to condensing steam is not created in any vessel or that the refinery fuel
gas system pressure is not appreciably reduced. Some additional fuel gas connections
may have to be made up to assist in the gas blanketing of the stabilizer and de-
isohexanizer. Pressure the stabilizer and de-isohexanizer up to approx. 0.7 kg/cm² g
with fuel gas.

g. Drain any residual condensate from the stabilizer and de-isohexanizer.
2.2 EVACUATING
Evacuating and nitrogen blanketing is normally the manner in which the reactor section is
freed of oxygen. For this section, the following guides are suggested:
♦ Test the Ejector (J-2301) to make sure that it will work. Line up and evacuate the
reactors through 2”-PG-230133.
♦ Make sure the gas flow will be in the same direction as the normal flow. This applies to
both the evacuation as well as the subsequent filling with nitrogen.
♦ Use a compound pressure gauge located as far as possible from the ejector.
♦ Following the final evacuation and fill, a portable combustibles analyzer should be used
to confirm that an explosive mixture does not exist (02 < 0.5 % vol).
♦ Do not evacuate any pumps. They are to be nitrogen purged separately.
2.3 NITROGEN PURGING

The liquid feed driers, the feed surge drum, the interconnecting lines, the methanator, the
make-up hydrogen driers and its associated equipment can be purged with nitrogen until
free of air. Leave this equipment under a slight positive pressure (N2) when the purging has
been completed. The best procedure for purging is by pressure-cycle purging, in which the
equipment is pressurized with an inert gas and then vented to atmosphere. The cycle is
repeated until the desired oxygen level is achieved, which should be less than 0.5 % vol.
NOTES: It is better to pressurize/depressurize 5 times up to 1 or 2 kg/cm² g each time, than
to pressurize/depressurize once up to 5 kg/cm² g. In the first case the theoretical
final oxygen content is 25 = 32 times less than the original one. In the second case
the theoretical final oxygen content is only 5 + 1 = 6 times less. Never exceed
system design pressure if safety valves are in service.
Purging can be speeded up by pulling a vacuum on the system before pressurizing.
However, attention must be paid to the equipment design before this operation may be
considered.
Under no circumstances should a vacuum be applied indiscriminably to equipment without
first checking that the equipment is capable of withstanding vacuum conditions.
During all purging and/or depressuring drain all low points of any water.
LOGIC DIAGRAM FOR START-UP SEQUENCES

METHANATOR
Section line up
Pressurize system with nitrogen
Start A-2302 and increase

temperature at T-2301 inlet to 231
°C
Slowly introduce hydrogen
Block in the nitrogen and pressure

unit up to 38.6 kg/cm² g
Check for CO at R-2301 outlet
Line out the column

Important: No CO/CO2 containing hydrogen should be introduced to the methanator below

149 °C because nickel carbonyl will form and can damage the catalyst by depleting the
nickel from the catalyst.
Proceed to Methanator start-up as follows:
a. Isolate Methanator system from downstream units by closing block valve on line 3”-PG-
230019.
b. Introduce nitrogen via 1”-N-230011 line and pressure the methanator system up to
nitrogen header pressure.
c. Start a nitrogen flow through the system by opening the 1½” block valve on the vent to
the flare 1½”-PG-230009.
d. Immediately commission the methanator heater and raise the outlet temperature to
231°C at the rate of 110°C/hour. Commission Methanator cooler E-2303 to ensure that it
is operational.
e. When the methanator outlet temperatures reaches 149°C, slowly introduce hydrogen
from the hydrogen plant via 1” bypass block valve on line 3”-PG-230001. As the catalyst
is normally supplied in an oxidized state, the introduction of hydrogen will start to reduce
the catalyst and a temperature rise will occur. A temperature wave will pass through the
catalyst. Limit the hydrogen to control a 28°C delta temperature rise. Hold 231°C on the
methanator inlet until the reduction has been completed. Close block valve on nitrogen
inlet line 1”-N-230011 and on vent to the flare 1½”-F-230010 and pressure up the
system slowly with hydrogen from the hydrogen plant. Control system pressure with PG-
030.
f. Open up the vent to the flare 1½”-F-230010 and establish a minimal hydrogen flow rate.
Check for CO at the methanator outlet. If <0.5 ppm, proceed. If not, raise the methanator
inlet by 6°C, equilibrate and check again.
g. Close the warm-up vent to the flare 1½”-F-230010 and begin hydrogen flow to the
Isomerization Unit by opening block valve on line 3”-PG-230019.
With the specified hydrogen gas flow, the delta T across the reactor may be very low or in
the case of H2 plant, H2 could be as high as 55°C. If there is no delta T, check for CO
conversion.
• If CO is present at the outlet, raise the reactor temperature again by 6°C and check
the CO conversion again.
• If no CO is present at the reactor outlet, check the CO at the inlet. The lack of delta
T may be due to a lack of carbon oxides in the makeup hydrogen gas.

With all of the process equipment purged of oxygen as verified by the refinery safety
department and under an inert gas blanket, the first phase of drying down the unit (initial
drydown) can begin.
4.1 WATER WASH NET GAS SCRUBBER AND CHLORIDE INJECTION

After leak test and inerting of net gas scrubber, establish 80% water level in T-2302,
indicated on LI-009A. Pressurize scrubber to 6 kg/cm² g with N2 indicated on PIC-024.
Commission Water Injection Package X-2304 as per Vendor’s Instructions and start Water
Injection Pump P-2309 A.
Establish 60% water level in T-2302 upper section, indicated on LI-017. When level is
established, start water circulation pump P-2308 A and establish minimum flow to the Net
Gas Scrubber T-2302 via FV-022. Maintain level in T-2302 upper section at 60% of LI-017.
Slowly increase the flow at FV-022 to 6000 kg/h with stable operation.
Prepare caustic circulation pumps for operation as per Pump Vendor Operating Instructions
(motor has been run uncoupled during electrical checks).
Start P-2307 A and establish minimum flow via FV-020 to the Net Gas Scrubber T-2302.
Maintain level in T-2302 at 60% of LT-009. During initial operation, close attention must be
kept on pumps. Checking bearing temperatures, seal flows and cavitation. Should cavitation
occur, stop the pump immediately and check the suction strainer.
Slowly increase the flow at FV-020 to 3,000 kg/h with stable operation via FV-020, start the
flow to the top of the scrubber via FV-021. Maintain a level in the scrubber by addition of
water from water injection package and through caustic transfer pump P-2306 A. Slowly
increase the flow via FV-021 to 7,000 kg/h. Alternate from pump A to B and check the
suction strainers. Continue with water circulation until suction strainers remain clean. Drain
water from system and charge 10 % wt fresh caustic (14.4% wt caustic from refinery header
diluted to 10% wt with water from Water Injection Package). Restart circulation as above.
CHLORIDE INJECTION
The level glass LG-800 of Chloride Injection Drum D-2302 should be calibrated for volume.
Using a measuring flask fill the level glass, making volume versus mm. The level glass is
used in the calibration of P-2303 A/B.
Prior to charging chloride, the equipment has been cleaned, dried and inerted. Put
blanketing N2 in service PCV-817 regulating at atmospheric pressure, PCV-815 at 1.76
kg/cm² (g) and PCV-816 at 2.11 kg/cm² (g). A 2” bypass valve is installed at PCV-816 for
truck or iso-container unloading.
Chloride is charged to D-2302 either from drums via Chloride Transfer Pump P-2302, or
from truck or iso-containers with 2" vent on Chloride Injection Drum D-2302.
4.2 REACTOR AND LINE SWITCHING

During this "Dryout" and the subsequent "Acidizing" period, it will be necessary to change
the flow pattern through all of the reactors and associated piping to ensure that all lines are
used. In addition any "dead" lines in the reactor circuit, e.g. control valve bypasses should
have flow established through them for a short time, also instrument lead lines are to be
purged. An operator is to be stationed at the CV bypass and instruments during this operation.
This line and reactor switching is done to ensure that no pockets of water (initial drydown) or
rust (acidizing) will remain in the system.
Initially line up the reactors for series flow operation. Then, every eight hours after
hydrocarbon circulation has been established, switch the flow pattern as follows:
♦ Reactor A single operation
♦ Reactor B single operation

♦ Reactor A to Reactor B series operation
♦ Reactor B to Reactor A series operation
When switching, make sure that flow through the system is always maintained and do not
proceed to the next step before completely opening or closing the valves listed in each step.
4.3 HYDROGEN ADDITION

Introduce hydrogen to the unit. The process flow will be lined up from battery limit (B.L.),
through Methanator R-2301, Make-up Gas Driers DR-2301/2302 in a series flow
configuration up to 3” block valve on line 3”-PG-230022. Pressurization should be done in a
stepwise manner, taking care not to disrupt the upstream unit. Rate of pressurization should
be controlled via 3" block valve at B.L. and pressure monitored at PG-065. At each stage of
pressurization leak checks should be carried out. Continue pressurizing until block valve at
B.L. is full open and the system is at make-up gas header pressure (42.3 kg/cm² g).
For pressurizing the section downstream of block valve, line up the Reactors R-2302/2303
in a series flow configuration up to PV-097. Again pressurization should be done slowly and
in a stepwise manner. Control rate of pressurization via 3” block valve and monitor upstream
pressure on PG-046 and PG-047 so as not to disrupt upstream unit. Once more carry out
leak checks at each stage of pressurization. Pay particular attention to thermocouple
flanges on reactors, as it will be very difficult to rectify leaks in these areas after catalyst is
loaded. Pressurize this section to 19 kg/cm² g as indicated on PG-047 and PIC-097.
The Stabilizer T-2301 and Stabilizer Receiver D-2303 will be pressurized via line 1½”-PG-
230096. Prior to pressurizing, ensure that P-2304 A/B suction and discharge valves are
closed. Pressurize and leak check as stated above, until 14.1 kg/cm² g, as indicated on PIC-
022 and PG-060.
When all three sections are pressurized, place PIC-097 in automatic at 19 kg/cm² g and
establish a minimum flow at FIC-013. As pressure in reactor section increased, PV-097 will
open to maintain setpoint pressure. Maintain stabilizer pressure at 14.1 kg/cm² g by venting
gas to flare header via 1½”-F-230189, located upstream PV-022. This action will purge the
system free of nitrogen, prior to passing the gas through the Net Gas Scrubber T-2302 and
the fuel gas system.
With caustic circulation established in the net gas scrubber, the gas can be transferred from
the flare header to the fuel gas system via the scrubber. Set PIC-022 in automatic with
setpoint at 14.1 kg/cm² g and PIC-024 in auto with setpoint at 6.3 kg/cm² g. Slowly close
1½” valve at 1½”-F-230189. As pressure increases PIC-022 will open passing the gas to
scrubber where the pressure will be controlled at 6.3 kg/cm² g by PIC-024 passing the gas to
the refinery fuel gas system.
4.4 HYDROCARBON ADDITION

The filling of the Liquid Feed Driers DR-2303/2304 must be done slowly, so that blanketing
gas can be purged from the vessels. The liquid feed driers can be filled in parallel via the 2"
filling lines on 6”-PL-230067 bypassing the remote operated valves at the DR-2303/2304
bottom inlets, through to the Feed Surge Drum D-2301. Crack open 4” feed valve at B.L. to
slowly fill DR-2303/2304, and establish a level in the feed surge drum D-2301. Monitor the
upstream pressure on PG-188, so as not to disrupt upstream unit. Establish operating level in
the feed surge drum. At this point Split Range Controller PIC-090 should be put into
operation with a setpoint of 6.2 kg/cm² g. Line up the feed driers in series, close 2" fill
valves.
Start P-2301 A as per Vendors instructions on circulation via FIC-007 start up spill back to
D-2301, maintaining a flow above the pump minimum flow requirement. During this initial
running of the pump, the pump should be monitored continuously. Run pump A for one
hour, then switch over to pump B for check of this pump. When both pumps have been
running satisfactorily, the feed can be charged to the stabilizer.
Feed is charged to the Stabilizer T-2301 via the start-up bypass line 4”-PZ-230130, which
bypasses the reactor section and ties into 6”-PZ-230370 downstream of the Reactor
Pressure Control Valve PV-097. The filling rate can be read on FIC-009. The level in the
feed surge drum should be watched in order to prevent losing feed pump suction. Flow to
stabilizer is controlled by FIC-009. Start one fan in Stabilizer Condenser E-2310. Check that
cooling water is in service to Stabilizer Trim Condenser E-2311. When a level appears in the
stabilizer bottom, line up MP steam to Stabilizer Reboiler E-2309. Increase heat input to
reboiler by slowly increasing MP condensate flow at FIC-016. When level appears in
Stabilizer Receiver D-2303, start P-2304 A and send reflux to the column. Adjust
condensate flow at FIC-016 to maintain level in Stabilizer Receiver D-2303, put LIC-008 in
automatic. Increase flow at FIC-016 to establish reflux flow of 8,500/9,000 kg/h. As the level
in the stabilizer increases, line up the bottoms to the De-isohexanizer (DIH) T-2303. Put the
DIH Condenser E-2317 in service. PIC-027 is set at 1.3 kg/cm² g. PDIC-028 set at 0.7
kg/cm² g.
NOTE: It will be necessary to vent non-condensables from DIH Receiver D-2306 during
start-up, this can be done via 2” bypass on PSV-017.
When a liquid level starts to accumulate in the column bottom, start MP steam to DIH
Reboiler E-2316. Heat up slowly to avoid tray damage due to the rapid vaporization of water
that may be in the column. Pay particular attention when the DIH bottoms temperature
reaches saturated steam temperature for the DIH bottoms pressure. Line up overhead and
bottoms to off spec storage during column lining out. Cooling water will already be in service
to E-2315 and E-2318. Start P-2311 A as per Vendors instructions and establish a flow via
FV-027 to DIH reboiler. The flow should be set at 2200 kg/h. Pump is now ready if required
to pump DIH bottoms to storage. When level appears in DIH receiver, start P-2312 A as per
Vendors instructions and send reflux via FV-034 to the column. Put LIC-015 in auto. Adjust
steam to reboiler to increase reflux flow above pump minimum flow requirement. Drain all
low points in DIH circuit, particularly DIH overhead receiver. Line out the column at
conditions near its normal operating temperature and pressure. Sample the DIH overhead
receiver. If the sample is clear and bright, it can be routed back to the feed driers via Start-
up Bypass 3”-PL-230255.
Increase feed and hydrogen rates slowly to establish stable operation at 50% of the design
reactor charge rate (25143 kg/h) and 100% of the design hydrogen flowrate ( 609 kg/h).
When column is on stable operation and liquid level is established on tray 71, commission
Deisohexanizer Side Draw Reboiler E-2312 and establish flow through reboiler via FV-025.
The flow should be set at 32150 kg/h.
At this time, instruments should be tuned and put in automatic/cascade where possible.
Calibrate the moisture analyzers in the unit and commission them to monitor drier
performance.
Initiate drier regenerators. See paragraph 10.3 of this chapter for information relating to drier
operations.
4.5 REACTOR CIRCUIT CIRCULATION

Slowly increase the reactor pressure to approximately 28 kg/cm² g via hydrogen purge line
3”-PG’230131. Place the reactor section on pressure control via pressure controller PIC-
097. Establish a flow of hydrogen make-up gas and increase the flow to design.
Drier regeneration and cooling should be completed before flowing through the reactors.
With 50% liquid feed and 100% gas rates stabilized throughout the unit, the reactors will be
heated up for preliminary drying.
Warm up and put in service MP steam to Charge Heater E-2308. Slowly warm up process
outlet temperature at TIC-056 to 121°C, by increasing flow of steam condensate at FIC-014.
Place TIC-056 – FIC-014 in cascade control. Interlock UX-004 feed and/or hydrogen low flow
shutdown will stop flow of condensate from E-2308.
With pressure and temperature control established throughout the unit, slowly reroute the
feed, which is flowing through the start-up bypass, so that it enters the reactor section
through the normal charge line. Slowly close start-up bypass to ensure flow to reactors.
During this period when the reactor section is being inventoried with hydrocarbon, feed will
be lost to the stabilizer and DIH. Pressure upsets are expected in the reactor section,
stabilizer and DIH. Therefore, just prior to the feed being routed to the reactor section,
reduce stabilizer heat input to Stabilizer Reboiler E-2309 by reducing flow of condensate at
FIC-016. Likewise at DIH Reboiler E-2316 via FIC-026. Maintain columns on reflux until
reactor section is inventoried.
When liquid feed is re-established to stabilizer and DIH, line out unit once more at 50%
liquid feed and 100% hydrogen rates, with DIH lined up to off spec storage.
Set PIC-097 in automatic at 31.7 kg/cm² g to raise reactor pressure up to normal operating
pressure by design. The liquid leaving the reactor section to the stabilizer contains the H2
makeup gas which will increase the pressure on the stabilizer.
Establish pressure control on the stabilizer at 14.1 kg/cm² g via PIC-022. The stabilizer
pressuring gas flow can be discontinued at this time.
With both reactors in service, hold the reactor inlet temperatures at a minimum of 177°C
(and higher if possible up to 204°C) by adjusting setpoints at TIC-056 and TIC-024.
The flow of liquid feed through the reactor section will remove the films of oil placed there
after sand blasting. Drier regeneration and cooling will be completed before flowing through
the reactors and then discontinued for the first eight hours after liquid feed flow has been
established in the reactors by shutting down the regeneration system and stopping the flow.
The timing of the initial liquid feed drying should be adjusted to fall between regeneration
cycles to avoid placing any of the oil contaminated liquid feed from the reactor circuit over
the drier material. The oil will flow out in the DIH column bottoms, which will be routed to off
spec storage via P-2311 A/B through DIH Bottoms Cooler E-2315 flow controlled by FIC-
028.
Moisture Analyzer AT-001 D is installed at the inter reactor sample pot to measure the water
content of the reactor effluent during start-up. Lead reactor samples via ¾”-PZ-230163, lag
reactor sample via ¾”-PZ-230134. This sample system should be well flushed during dry out
to obtain accurate moisture readings.
During this hydrocarbon circulation it will be necessary to alter the flow through the reactors
and the reactor circuit piping as outlined previously in reactor and line switching. The sulfur
stripping lines 3”-PG-230150, 3”-PG-230047 and 3”-PG-230050 and hydrogen quench lines
should also be dried out during this period.
Continue drying until the water content of the liquid leaving the reactor is below 10 ppm wt
(see Figure 4.5.1).
Figure 4.5.1

When the water content in the system has been reduced to the level of less than 10 ppm wt,
injection of anhydrous HCl will be initiated to remove any iron oxide not removed by the
sand blasting.
♦ Drain any liquid water that may have accumulated in the stabilizer overhead receiver and
DIH receiver. During the acidizing period with HCl it will be necessary to check and drain
this point on a frequent basis as a highly acidic liquid could be present.
♦ The stabilizer off gas scrubber is in service circulating 10 % wt caustic solution.
♦ Connect up the cylinder of anhydrous HCl to the inlet of the Cold Combined Feed
Exchanger E-2306. The cylinder of HCl should be mounted on a scale such that an
injection rate determination can be made (see Figure 5.1).
♦ During the acidizing period it will be necessary to temporarily block in the Moisture
Analyzer AT-001 D on the inter-reactor sample pot during the HCl injection as the highly
acidic environment could damage the analyzer probe. After HCl has been injected, an
hour period will be allowed to lapse and then the analyzer will be recommissioned if the
HCl content of the gas from the inter-reactor sample pot is less than 10 ppmv (see
Figure 5.2).
♦ With hydrogen and hydrocarbon flow established in the unit and drier regenerations
being performed frequently, the following will outline the acidizing and final drydown
steps.
a. Block in the moisture analyzer probe that is monitoring the reactor effluent AT-001 D.
b. Inject 5 kg of HCl to the system over a 10 minute period of time.
c. Wait one hour with unit circulation continuing or until the reactor effluent sample pot
vapor contains less than 10 ppmv of HCl.
d. Reconnect the moisture analyzer and obtain a reading on the sample pot liquid.
e. Continue injecting HCl (repeat steps "a" through "d") until the moisture in the reactor
effluent liquid reaches a maximum and starts down. During this period continue
draining low points, purging instrument lead lines, flushing by-passes around control
valves and switching the reactor flow pattern. The sulfur stripping lines and hydrogen
quench line should also be acidized during this period during a shift.
f. When no further unit response to HCl addition is noted by the moisture analyzer, have
the instrument department verify that the readings are correct. Add another 12 kg of
HCl over a half hour period. Again re-check the moisture content of the effluent stream.
If no response is noted, discontinue HCl injection and dry the unit down (continue unit
circulation) until the reactor effluent is 1 ppm wt. If a response to this last HCl addition
is noted, then return to step "a".
g. It is typical to inject the design quantity of HCl. If no iron oxide is present, additional
injection of HCl consumes the HCl and caustic; however, unit final drydown is initiated
which does not impact the overall start-up schedule.
See Figure 5.3.
♦ It will be required to run the C2Cl4 injection pumps at this time and carry out the injection
pump calibration if it has not been done before.
♦ Reduce and eventually stop the flow of steam to the Charge Heater E-2308. Continue
liquid feed and hydrogen flow through the reactor circuit until the reactors have been
cooled to 121°C.
♦ When the reactors have been cooled to 121°C, again route the liquid feed through the
start-up bypass.
♦ Continue make-up gas H2 flow to the unit such that the pressure on the stabilizer can be
temporarily maintained.
♦ Sweep the entire reactor circuit with the hydrogen to purge all of the hydrocarbon over to
the stabilizer.
♦ Cool the reactor circuit to 49°C.
♦ Discontinue make-up hydrogen addition and keep pressure on the reactor section.
♦ Block in each of the reactors, inlet and outlet, and blind the reactors.
♦ If liquid feed circulation becomes unstable at this time (i.e., loss of pressure on the
stabilizer), it might be advantageous to discontinue it.
♦ Depressure, evacuate and purge each reactor. Use dry nitrogen containing less than 10
ppm of water for the purge. If this is in doubt, route the nitrogen through a freshly
regenerated, properly purged hydrogen drier. Clean temporary piping will be needed for
this operation. No refinery hoses will be used. Perform the evacuation and purging
operation twice. Maintain a positive nitrogen pressure on the reactors.
♦ Maintain hydrogen pressure on the balance of the reactor circuit.
♦ The isomerization reactors are now ready for loading. Proceed to the I-8 Plus/I-82
Catalysts Loading Procedure.
Figure 5.1
Figure 5.2
Figure 5.3
6. CATALYST LOADING
6.1 LOADING VESSEL SUPPORT MATERIAL

The loading of the reactors will take place in two distinct stages. The first is the installation
of the catalyst support material before the unit is dried and the second is the actual catalyst
loading after the unit has finally been dried. Only the first phase will be presented at this
time.
a. With the completion of the sand blasting and oil coating, the reactors are ready for the
installation of the catalyst support materials.
b. Install the slotted cap over the bottom outlet. Check to ensure there is a good fit in order
to avoid passage of ceramic support between the bottom of the basket and the outlet
nozzle.
c. The support plates should be installed in the unloading nozzles and a coil of 13 mm
diameter ceramic fiber rope laid over them.
d. Install the sleeves in the unloading nozzles and fill with 6 mm balls to 100 mm from the
top. Add 100 mm of 3 mm diameter balls.
e. For the loading of the ceramic support, the upper manhole should be used. The balls
lowered by rope and bucket.
f. With the bottom internals in place, load 19 mm diameter balls up to a height of 330 mm
above bottom tangent line. The top of this layer should be leveled.
g. A 100 mm of 6 mm diameter balls is loaded on top of the 19 mm diameter balls, taking
care not to disturb the 19 mm balls. The top of the 6 mm layer to be leveled.
h. A 100 mm layer of 3 mm diameter ceramic balls is loaded on top of the 6 mm balls,
taking care not to disturb the lower layer and making sure each layer remains leveled.
i. Install the thermocouples. Ensure that thermowells project sufficient length into reactor.
Ensure flange faces are clean and correct rating gaskets installed.
j. Install vapor/liquid distributor tray and inlet distributor and head up the reactors.
See also Figures 6.1 and 6.4
6.2 I-8 PLUS / I-82 CATALYSTS LOADING

The following outlines the general procedures to be used for loading the reactors. A mixed
phase PENEX reactor loading diagram is outlined in Figure 6.1. The I-8 Plus and I-82
catalysts are dense loaded. UOP recommends the reactors be dense loaded using the UOP
Inert Dense Loading Technique if there is a liquid and vapor phase present in the reactors.
This recommendation is made to ensure good flow distribution throughout the catalyst bed.
If the unit was designed with a vapor and liquid distributor tray inside the reactor (in addition
to the inlet distributor) the catalyst should be dense loaded. For details of the UOP Inert
Dense Loading Device, the UOP Dense Loading Coordinator should be contacted at the
following address:
UOP Dense Loading Coordinator
UOP
25 East Algonquin Road
Des Plaines, IL 60017-5017
USA
The catalyst loading procedure follows:

6.2.1 GENERAL
There are problems, which are inherent to accomplishing reactor catalyst loadings, and it is
therefore beneficial that the following procedures and details be thoroughly understood by
everyone who will be associated with the job prior to actual loading.
a. As the reactor circuit has been acidized to remove mill scale and has been dried
especially well, care must be taken to ensure that no air or moisture enters the
reactor circuit during the catalyst loading period.
b. The I-8 Plus / I-82 Isomerization Catalysts are shipped in sealed 55-US gallon drums
that have a special protective lining (refer to Figure 6.2.1 in Chapter 5). The catalysts
are contained in a heavy plastic bag with a long neck. The neck is crimped in two
places with wire and heat-sealed at the end. This bag is inside another heat-sealed
plastic bag.
c. Before, during and after catalyst loading, the catalyst must be protected from
moisture at all times. Any contact with water or air will result in permanent
deactivation of the catalyst.
d. Rough handling of the catalyst drums should be avoided since the heat seals on the
plastic catalyst bags could be broken. Care should be taken not to damage the empty
drums because they will be used to return spent catalyst for platinum recovery.
e. The catalyst must be loaded into the reactors directly from the 55-US gallon drums.
No other temporary loading hoppers may be used due to the water sensitivity of the
catalyst.
6.2.2 EQUIPMENT AND MATERIALS REQUIRED

Prior to the loading of the reactors with catalyst, the following will be required:
a. Fresh UOP I-8 Plus and I-82 catalysts.
b. Catalyst loading assembly and UOP Dense Loading Device.
c. Loading sock.
d. Special unloading lids (two required).
e. Bailing wire.
f. Plastic sheeting.
g. Wire rubber bands - to fit a 6" diameter tube or surgical tubing.
h. Quick release drum lid retainer rings (two required).
i. Ample dry nitrogen (less than 5 ppm H2O).
j. Knife.
k. Tools to open catalyst drums.
l. Grounding wire.
m. Masking tape (2 to 3 inches in width).
n. Low range pressure gauge (0-10 inches H2O).
o. Dry hoses for nitrogen purging.
p. Dried ceramic balls for catalyst hold-down material.
q. Measuring tape to determine outages on reactor.
r. Two sets of air masks, harnesses, rope and other safety equipment for person
entering the reactor.
s. Metal sling for hoisting catalyst drums.
t. New gaskets for flanges and manways which were opened.

u. Shovel or scoop for leveling the catalyst bed (handle should be at least 2.5 meters).
v. Scissors to cut the heat seal on the loading neck of the plastic catalyst bag.
w. A light, suitable for a hazardous atmosphere, that will fit through pressure relief door
opening.
x. GOOD WEATHER.
6.2.3 CATALYST LOADING EQUIPMENT DETAILS
6.2.3.1 CATALYST LOADING ASSEMBLY

The attached figures represent the special loading assembly that is required to load the I-8
Plus and I-82 Isomerization Catalysts. As the catalyst is sensitive to both air and moisture,
there should be no deviation from what is specified in the drawings.
a. To conserve nitrogen, a soft rubber gasket should be glued to the bottom side of the
catalyst loading assembly. The pressure relief door should also fit tightly against the
assembly.
b. The top edge of the 6" loading adapter should have no sharp edges or corners to
reduce the chance of tearing the loading neck of the plastic catalyst bag.
c. The location of the UOP Dense Loading Device is indicated in Figure 6.2. The
dimensions of the sock attachment from the loading assembly to the UOP Dense
Loading Device vary from unit to unit, as do details of the device itself. These details
will be furnished by the UOP Dense Loading Coordinator.
6.2.3.2 LOADING SOCK

The catalyst will be transferred from the loading assembly to the dense loader using a
canvas sock. The sock should be secured to the bottom of the loading assembly and extend
of a length of 12 inches below the top of the dense loading hopper. The dense loading
device will be mounted on the top manway of the liquid/vapor mixing tray. The loading sock
will simply hang inside the dense loading hopper.
6.2.3.3 DRUM UNLOADING LID

The special drum lid, which will be required for the loading of the I-8 Plus and I-82 catalysts,
is shown in Figure 6.2.1 in Chapter 5. For the ease of loading and to load in an efficient
manner, there should be two of these lids available.
6.2.4 LOADING PROCEDURES
6.2.4.1 REACTOR OPENING

a. For the initial catalyst loading, the reactor should be in shutdown status. In case the
reactor section is not shutdown, the unit should be shutdown, following the normal
shutdown procedure.
b. Block in the reactor to be loaded, using the double block and bleed valves.
c. Depressure the reactor to flare.
d. Connect the reactor ejector and evacuate the reactor to 25 inches of mercury. Break the
vacuum with nitrogen to 0.35 kg/cm² g, then repeat the evacuation and pressuring.
Minimize the time at which the reactor is under a vacuum.
NOTE: The nitrogen used for breaking the vacuums and gas blanketing the reactor, should
contain less than 5 ppm water. If there is any doubt about the water content of the nitrogen,
it can be dried by passing it through one of the make up hydrogen driers using temporary
piping.
e. The nitrogen for breaking the vacuums should be connected to the reactor inlet.
f. Start a small purge of nitrogen into the reactor and out the 1” purge vent on line 3”-PG-
230050. Unbolt and remove the reactor inlet elbow and top head. As the reactor is
opened, tightly cover the open flanges with plastic. When the reactor inlet elbow is
removed, wrap it and the inlet distributor in plastic and immediately install the catalyst
loading assembly. The loading assembly should be installed on the top manhole and the
loading sock extended to just below the liquid/vapor distribution tray (refer to figure 6.3).
g. Connect the nitrogen hose to the loading assembly. Throughout the loading a separate
nitrogen purge to the reactor should be maintained through the hardpiped nitrogen
connection. Ensure that a positive pressure of nitrogen is maintained on the reactor
during the loading. 1-2 inches of water on the low range pressure gauge will suffice.
h. The dense loader is mounted on the V/L tray (refer to Figure 6.2), the loading assembly
should be attached to the top manhole. The loading sock should fit inside the dense
loader hopper. The nitrogen connection for the dense loader motor and the tachometer
connection should be made before the loading assembly is installed on the top manhole.
i. Ground the loading assembly and adapter to the reactor and connect the loading sock
grounding wire to the reactor.
NOTE: AT NO TIMES SHOULD A PERSON ENTER A REACTOR HAVING A NITROGEN
PURGE ON IT WITHOUT FULL INSTRUCTION AND EXPERIENCE WITH A FRESH AIR
MASK, SAFETY HARNESS AND LIFE LINE.
6.2.4.2 CATALYST LOADING

1. At ground level
Remove the drum lid and open the outer (heavy) plastic bag.
Install the special loading lid with the 150 mm hole using a “quick release” lid retaining ring.
Pull the loading neck of the inner plastic catalyst bag through the hole. DO NOT remove the
wire clips or break the heat seals on the loading neck.
Position the drum for hoisting to the top of the reactor with the drum horizontal and the 150
mm hole in the lid oriented downward.
NOTE: NO MORE THAN TWO DRUMS ARE TO BE OPEN AT ANY TIME AT GROUND
LEVEL, one drum ready to be hoisted and one drum being prepared.
2. At the reactor
Hoist the drum to the reactor and position the drum for loading.
Cut the heat seal on the loading neck close to the seal and slip the neck over the adapter.
Hold or secure the neck with a web band or surgical tubing.
Remove the wire clamps on the loading neck and start to load the catalyst. Securely hold
the neck so that the heat seals on the sides of the neck do not break during the loading.
Adjust the nitrogen flow to the dense loader motor to achieve the correct RPM’s. When most
of the catalyst has been loaded, start to gently pull the plastic bag and remaining catalyst
through the hole in the lid until the bag is removed from the drum and all of the catalyst has
been loaded. It is not necessary to remove the lid as the inner bag can be pulled through the
hole as the bag is emptied.
It will be necessary to stop the loading 3 or 4 times to check the surface of the catalyst bed
to ensure that the catalyst is being loaded properly. To do this, the loading assembly must
be removed from the reactor manway to allow an inert entry specialist to enter the reactor to
make an observation. Based on the condition of the surface of the bed, the dense loading
RPM’s will be adjusted.
Return the drum, plastic bags and loading lid to the ground level. Keep the adapter on the
loading assembly covered when loading is not in progress to conserve on nitrogen.
3. Finish of loading
After the last drum of catalyst has been loaded, per the reactor loading diagram, hoist the
drum of hold-down balls to the reactor. An inert entry specialist must remove the dense
loader and level the catalyst bed with a scoop or shovel. After apour d the bed, check
the outage to the catalyst.
Using buckets, load the hold-down balls into the reactor. First, load 100 mm of 6 mm
diameter balls. Level the layer and then load 100 mm of 19 mm diameter balls and level the
layer.
A nitrogen purge into the reactor upper head is maintained throughout these final loading
steps.
After the last layer of ceramics is apour d and the apour/liquid tray manway is
reinstalled, then cover the manhole with plastic once the inert entry specialist leaves the
reactor.
6.2.4.3 REACTOR CLOSING

1. As quickly as possible after the loading is completed, install the inlet distributor, ceramic
fiber rope, reactor head and inlet elbow.
2. Continue the nitrogen purge to the top of the reactor and purge out the bottom to flare.
Check that the purge gas at the reactor outlet is below refinery standards for admitted
hydrocarbons and is free of oxygen. Pressure the reactor to 0.35 kg/cm² g. Disconnect,
blind plug all nitrogen purge lines.
NOTE: The opening, loading and closing of the reactors should be a continuous operation
with no breaks. During the opening, loading and closing of the reactors, a dry nitrogen
blanket MUST be maintained at all times.
Figure 6.1
Figure 6.2
Figure 6.3
Figure 6.4
7. INITIAL START-UP
Upon completion of the catalyst loading operation, the reactors can be prepared for start-up.
Initially only one reactor will be placed on line.
When feed is first introduced to a reactor, particularly when the catalyst is fresh, it is
important that the severity of operation be minimized to prevent hydrocracking and the
resulting high reactor temperatures. It is very important that the procedure be followed
exactly as detailed below. No alterations will be accepted by UOP.
The logic diagrams for start-up sequences of the net gas scrubber and the Penex process
unit are attached.

NET GAS SCRUBBER
TIGHTNESS TEST, I-8 PLUS / I-82 CATALYSTS LOADING AND

BLANKETING COMPLETED. UNIT IS UNDER INERT GAS
PRESSURE
Section Line up
Pressurize T-2302 with nitrogen to

about 6 kg/cm² g
14.4% wt caustic available from

refinery header
Start Water Injection Package

X-2304
Establish level in T-2302
Start P-2307 A/B
Adjusting T-2302 reflux rates


PENEX PROCESS UNIT
TIGHTNESS TEST, I-8 PLUS / I-82 CATALYSTS LOADING AND

BLANKETING COMPLETED. UNIT IS UNDER INERT GAS
PRESSURE
Section Line up
Pressurize R-2302/2303 with

nitrogen to about 28 kg/cm² g
Pressurize T-2301 to normal

operating pressure of 14.1 kg/cm² g
Establish H2 makeup flow and

increase to design condition
Charge Heater E-2308 in operation
Introduce feed to R-2302/2303

Reactor temperature not above
65°C

PENEX PROCESS UNIT
Route feed to T-2301 and stabilize

the operation
Increase R-2302/2303 inlet

temperature to 121°C
Start Chloride injection
Raise R-2302/2303 effluent pressure

to 31.7 kg/cm² g
Line out the unit

7.1 INITIAL OPERATION

The reactors will be pressure tested in parallel.
NOTE: Upstream and downstream equipment is still pressurized.
a. Slowly increase the pressure in the reactors in a stepwise method to 28 kg/cm² g.
This "pressure up" is accomplished by opening the line 3”-PG-230131 via the 1½”
globe valve to reactor inlet lines 6”-PZ-230137 and 6”-PZ-230139. With the globe
valve the pressure-up rate can be controlled. Leak checking all flanges that were
opened during catalyst loading.
b. Once the reactors have been pressure tested, line up the lead reactor for operation.
The lead reactor effluent will be lined up to completely bypass the Hot Combined
Feed Exchanger E-2307 A and B by opening TV-024 B and closing TV-024 A. The
lag reactor will be bypassed, using the "single reactor operation" bypass 6”-PZ-
230140.
c. Pressure up the Stabilizer T-2301 to the normal operating pressure of 14.1 kg/cm² g
on PIC-022. Use the pressurizing line 1½”-PG-230096 from the hydrogen driers to the
stabilizer. Excess stabilizer off gas is to be routed through the Net Gas Scrubber T-
2302, which should be in operation.
d. Establish hydrocarbon circulation as outlined in Section 6.3.4 Hydrocarbon addition.
Verify that the liquid feed driers are functioning, i.e., the moisture analyzer reads
below 0.1 ppm wt H2O. On start-up, the feed will be introduced to the reactor at least
50% of design. The reactors should never be operated at less than 50% of design
feedrate.
e. Raise the reactor circuit outlet pressure to 28 kg/cm² g with Reactor Effluent Pressure
Controller PIC-097. Verify that the make-up driers are functioning, i.e. the moisture
analyzer reads below 0.1 ppmv H2O.
f. Establish a flow of H2 make-up gas and increase the flow to design of 330 to 610
kg/h. It is very important that the make-up gas flow be at least design at the time feed
is introduced to the reactor.
g. Commission the Charge Heater E-2308 to ensure that it is operational. A very small
flow of steam to the heater should be maintained to ensure operability. Feed will be
introduced to the reactor cold. The heater is being commissioned at this point, rather
than after feed is cut in, to ensure that the heater functions properly. If the heater
does not function properly when feed is introduced, overheating of feed may result
and a reactor temperature excursion could occur.
h. With make-up gas flow and reactor pressure control established, prepare to introduce
feed to the reactor. FEED SHOULD NOT BE INTRODUCED TO THE REACTOR IF
ANY TEMPERATURE IN THE REACTOR IS OVER 65°C. Introduce feed to the
reactor by opening the block valves to the reactor circuit on line 6”-PZ-230126 and
closing the start-up bypass on line 4”-PZ-230130. Ensure that the feed is introduced
at a rate of at least 50% of design. This should be done as quickly as possible. Do not
try to maintain flow through the start-up bypass with feed going to the reactor. The
stabilizer and de-isohexanizer can operate on total reflux for the period of time that it
takes to inventory the reactor circuit.
i. When feed enters the reactor, there will be an exothermic reaction, which will
increase the reactor temperature quickly. This phenomenon will be short in duration.
The extent of the temperature increase will depend on the feed quality, however, the
rise should not cause a problem if the feed introduction temperature is lower than
65°C. Under no circumstances should the feed be removed from the reactor during
this initial start-up period unless the reactor temperatures increase above 232°C. This
will result in over-conversion of the feed and hydrocracking. If the temperature gets
over 232°C, the "High Reactor Temperature Differential Emergency" procedure
should be followed (see Chapter 6 §3.3).

j. Route the liquid feed to the stabilizer on pressure control. At this point, the entire unit
will be in operation at about 50% of design HCBN flow and 100% of design hydrogen
flow.
k. After stabilizing the operation, slowly increase the reactor inlet temperature to 121°C.
Raise the temperature at a rate of 11-17°C per hour via TIC-056. When the
temperature reaches 105°C, start the C2Cl4 injection. Inject C2Cl4 at 300 ppm wt (as
chloride) based on the reactor liquid charge. On a 50% of design HCBN flow the
injection rate is 4.8 L/h to be measured with LG-800 and controlled by stroke
adjustment of P-2303. When the first reactor stops consuming chloride, as
determined by stabilizer off gas chloride analysis, the chloride injection rate can be
reduced to 150 ppm wt. On a 50% of design HCBN flow the injection rate is 2.4 L/h.
Chloride breakthrough is typically observed within 24-36 hours of initial start-up on
fresh catalyst.
l. Raise the reactor effluent pressure to the normal operating pressure of 31.7 kg/cm² g
with PIC-097.
m. Route de-isohexanizer to product storage when on spec. The liquid leaving the
reactor section to the stabilizer contains hydrogen and light ends, which will increase
the pressure on the stabilizer. Establish pressure control on the stabilizer at the
design pressure. Discontinue flow of pressurizing gas from the make-up gas driers to
the stabilizer.
n. Continue lining out flow rates, temperatures, pressures, etc., throughout the unit.
o. Adjust the reactor temperatures to give the desired product ratio of approximately 70
IC5/C5P.
p. The Hydrogen Analyzer AI-003 on the scrubber off gas should be commissioned. This
signal is used to manually adjust the make-up gas rate such that a minimum of 0.05
H2/HCBN by weight ratio is maintained at the lag reactor outlet.
7.2 SERIES FLOW OPERATION

The first reactor should run for at least 2 days and stable normal operation verified before
the second reactor is put on line. The second reactor will be lined up such that it is in series
with the first reactor.
a. The off line reactor is at 28 kg/cm² g pressure. If not, pressure up the other reactor in
the same manner that was used for the on-stream reactor, i.e. via the "pressuring up"
line 3”-PG-230131.
b. The second reactor should be put on line with at least 50% of design feed to the first
reactor.
c. Reduce the reactor system pressure to 28 kg/cm² g at PIC-097.
d. Reduce the lead reactor outlet temperature to 121°C.
e. Establish flow of lead reactor effluent through the Hot Combined Feed Exchanger E-
2307 A and B and cool the feed to the lag reactor as much as possible. Transfer flow
from TV-024 B to TV-024 A slowly, so as not to upset control of TIC-056.
f. Open the off line reactor's inlet valves.
g. Open the off line reactor's outlet valves.
h. Establish flow through the reactor by closing the "single reactor operation" bypass
block valve at 6”-PZ-230140. Keep the lag reactor as cool as possible until the reactor
has inventoried and operations are stable.
i. When the second reactor is commissioned, the fresh catalyst will consume chloride
for a period of time. The chloride injection rate should be increased to 300 ppm wt
chloride based on feed in the same manner as for the first reactor. With 50% of the
design HCBN flow the injection rate is 4.8 L/h. This can be measured with LG-800
and controlled by stroke adjustment of P-2303. Reduce the chloride injection to 150
ppm wt based on feed after the chloride level in the stabilizer off gas levels off.
j. Raise the lag reactor effluent pressure to the normal operating pressure of 31.7
kg/cm² g with PIC-097.
8. NORMAL START-UP
The following procedures may be used to start-up the unit provided moisture and/or air was
kept out of the reactor section while shutdown. If air or moisture contaminated or is
suspected to have contaminated the reactor section, the dry-out, acidizing procedures and
initial start-up should be followed as provided in Chapters 6.4 and 6.7.
Two start-up procedures are given below. If the entire unit was shutdown then Chapter 6.8.1
should be used. If one reactor is in operation and the other reactor has just been loaded
with fresh I-8 Plus / I-82 catalysts, Chapter 6.8.2 should be used. Chapter 6.7.2 can also be
used to bring the second reactor on stream if one reactor was shutdown for a reason other
than catalyst change-out.
8.1 START-UP AFTER TOTAL UNIT SHUTDOWN

At this point it is assumed that the unit is shutdown and under a slight positive pressure of
H2 or dry N2.
a. Slowly increase the pressure in the reactors in a stepwise method to 28 kg/cm² g.
This "pressure-up" is accomplished by opening the line 3”-PG-230131 via the 1½”
globe valve to the reactor inlet lines 6”-PZ-230137 and 6"-PZ-230139. With the globe
valve the pressure-up rate can be controlled. Leak checking all flanges that were
opened during catalyst loading.
b. Once the reactor circuit has been pressure tested, line up the lead reactor for
operation. The lead reactor effluent will be lined-up to completely bypass the Hot
Combined Feed Exchanger E-2307 A and B by opening TV-024 B and closing TV-
024 A. The lag reactor will be bypassed using the "single reactor operation" bypass
6”-PZ-230140.
c. Pressure up the Stabilizer T-2301 to the normal operating pressure of 14.1 kg/cm² g
on PIC-022. Use the pressurizing line 1½”-PG-230096 to a point upstream of the
Stabilizer's Pressure Controler PIC-022. Excess stabilizer off gas is to be routed
through the Net Gas Scrubber T-2302, which should be in operation.
d. Establish hydrocarbon circulation as outlined in Section 6.3.4. However, route all
stabilizer bottoms - via the DIH T-2303 - to off spec storage. Verify that the liquid feed
driers are functioning, i.e. the moisture analyzer reads below 0.1 ppm wt H2O. On
start-up, the feed will be introduced to the reactor at least 50% of design. The
reactors should never be operated at less than 50% of design feedrate.
e. Verify that the make-up dryers are functioning, i.e. the moisture analyzer reads below
0.1 ppmv H2O. Establish a flow of H2 make-up gas and increase the flow to design. It
is very important that the make-up gas flow be at least design at the time feed is
introduced to the reactor.
f. Commission the Charge Heater E-2308 to ensure that it is operational. A very small
flow of steam to the heater should be maintained to ensure operability. Feed will be
introduced to the reactor cold. The heater is being commissioned at this point, rather
than after feed is cut in, to ensure that the heater functions properly. If the heater
does not function properly when feed is introduced, overheating of feed may result
and a reactor temperature excursion could occur.
g. With make-up gas flow and reactor pressure control established (PIC-097 in AUTO),
prepare to introduce feed to the reactor. FEED SHOULD NOT BE INTRODUCED TO
THE REACTOR IF ANY TEMPERATURE IN THE REACTOR IS OVER 65°C.
Introduce feed to the reactor by opening the block valves at 6”-PZ-230126 to the
reactor circuit and closing the start-up bypass 4”-PZ-230130. Ensure that the feed is
introduced at a rate of at least 50% of design. This should be done as quickly as
possible. Do not try to maintain flow through the start-up bypass with feed going to
the reactor. The stabilizer and de-isohexanizer can operate on total reflux for the
period of time that it takes to inventory the reactor circuit.
h. When feed enters the reactor, there will be an exothermic reaction, which will
increase the reactor temperature quickly. This phenomenon will be short in duration.
The extent of the temperature increase will depend on the feed quality, however, the
rise should not cause a problem if the feed introduction temperature is lower than
65°C. Under no circumstances should the feed be removed from the reactor during
this start-up period unless the reactor temperatures increase above 232°C. This will
result in over-conversion of the feed and hydrocracking. If the temperature gets over
232°C, the "High Reactor Temperature Differential Emergency" procedure should be
followed. (See Chapter 6 §3.3).
i. Route the liquid feed to the stabilizer on pressure control. At this point, the entire unit
will be in operation at about 50% of design HCBN flow and 100% of design hydrogen
flow.
j. After stabilizing the operation, slowly increase the reactor inlet temperature to 121°C.
Raise the temperature at a rate of 11-17°C per hour via TIC-056. When the
temperature reaches 105°C, start the C2Cl4 injection. Inject C2Cl4 at 300 ppm wt (as
chloride) based on reactor liquid charge. On a 50% of design HCBN flow the injection
rate is 4.8 L/h to be measured with LG-800 and controlled by stroke adjustment of P-
2303. When the first reactor stops consuming chloride, as determined by stabilizer off
gas chloride analysis, the chloride injection rate can be reduced to 150 ppm wt.
k. Raise the reactor effluent pressure to 31.7 kg/cm² g on PIC-097.
l. Route de-isohexanizer to product storage when on spec. The liquid leaving the
reactor section to the stabilizer contains hydrogen and light ends, which will increase
the pressure on the stabilizer. Establish pressure control on the stabilizer at the
design pressure. Discontinue flow of pressurizing gas from the make-up gas driers to
the stabilizer (1½”-PG-230096).
m. Continue lining out flow rates, temperatures, pressures, etc., throughout the unit.
n. Adjust the reactor temperatures to give the desired product ratio of approx. 70
IC5/C5P.
o. The Hydrogen Analyzer AI-003 on the scrubber off-gas should be commissioned.
This signal is used to manually adjust the make-up gas flow rate such that a minimum
of 0.05 H2/HCBN by weight ratio is maintained at the lag reactor outlet.
8.2 START-UP AFTER PARTIAL CATALYST CHANGE-OUT OR SHUTDOWN

The first reactor should run for at least 2 days and stable normal operation verified before
the second reactor is put on line. The second reactor will be lined up such that it is in series
with the first reactor.
a. Pressure up the other reactor in the same manner that was used for the on-stream
reactor, i.e. via the "pressuring-up" line 3”-PG-230131.
b. The second reactor should be put on line with at least 50% of design feed to the first
reactor.
c. Reduce the reactor system pressure to 28 kg/cm² g at PIC-097.
d. Reduce the lead reactor outlet temperature to 121°C.
e. Establish flow of lead reactor effluent through the Hot Combined Feed Exchanger E-
2307 A and B and cool the feed to the lag reactor as much as possible, by opening
slowly TV-024 A and closing TV-024 B.
f. Open the off line reactor's inlet valves.
g. Open the off line reactor's outlet valves.
h. Establish flow through the reactor by closing the "single reactor operation" bypass 6”-
PZ-230140. Keep the lag reactor as cool as possible until the reactor has inventoried
and operations are stable.

i. When the second reactor is commissioned, the fresh catalyst will consume chloride
for a period of time. The chloride injection rate should be increased to 300 ppm wt
chloride, based on reactor liquid charge in the same manner as for the first reactor.
On a 50% of design HCBN flow the injection rate is 4.8 L/h, measured with LG-800
and controlled by stroke adjustment of P-2303. Reduce the chloride injection to 150
ppm wt, based on feed after the chloride level in the stabilizer off gas levels off. On a
50% of design HCBN flow the injection rate is 2.4 L/h.
j. Raise the lag reactor effluent pressure to the normal operating pressure of 31.7
kg/cm² g with PIC-097.
9. DE-ISOHEXANIZER START-UP

DEISOHEXANIZER
Column is air freed and under fuel

gas pressure
Establish liquid level in T-2303
Start heat to DIH reboiler E-2316
DIH condenser E-2317 in service
Establish liquid level in D-2306
Start P-2312 and T-2303 on total

reflux
Start flow to E-2312
Line out the column

When the column is air freed and under fuel gas pressure, light straight run (LSR) naphtha
may be brought into the DIH section. Prior to doing this, ensure that all low points in the
system have been drained of condensate.
Proceed to DIH start-up as follows:
a. Establish a liquid level in the DIH T-2303 by transferring some fresh LSR feed to the
column from the isomerization unit's stabilizer discharge of bottoms to the DIH feed
line. Line up net overhead and bottoms to off spec feed storage during column line
out period, or maintain total column circulation by blocking in DIH overhead and
bottoms products.
b. When liquid starts accumulating in the column bottoms, start heat to the DIH Reboiler
E-2316 and begin heating the column bottoms liquid. Heat up slowly (± 10°C/h), to
avoid tray damage due to rapid vaporization of water that may be in the column. Pay
particular attention when the DIH bottoms temperature reaches saturated steam
temperature for the DIH bottoms pressure.
c. Ensure that the DIH Condenser E-2317 is in service. Commission the DIH Pressure
Controllers PIC-027 and PDIC-028.
NOTE: It may be difficult to line out the column at this point, due to non-condensable gas. Vent
receiver to maintain pressure as required, via Bypass PSV-017.
d. When a liquid level is established in the DIH Receiver D-2306, commission the DIH
Overhead Pumps P-2312 A/B and put the DIH on total reflux.
e. Start flow to side draw reboiler E-2312. Line out the column at conditions near to its
normal operating temperature and pressure.
NOTE: As required, introduce more naphtha from the stabilizer bottoms to the DIH to maintain
a reasonable liquid level in the DIH during the warming-up operation.
f. Once on spec product is made, divert net products to storage.
The logic diagram for start-up sequence of the deisohexanizer is attached

In the following sections guidelines are given to operate the unit in normal conditions. It also
includes recommendations for correction of deviations of the main parameters from normal
values. In the following sections alarm settings are mentioned, however, these values could
change as the result of gained operating experience. Therefore, always refer to the alarm-
sensing summary for the actual data.
Operating conditions present in the heat and material balances and on the process flow
diagrams (PFD's) reflects the normal operating conditions.
Furthermore, this chapter includes a typical example for collecting data & quality control.
As in any chemical process the isomerization unit has many operating variables which
influence product purity, yields, utility consumption etc. The process specification for this
unit is used only as a guide as reduced rates, equipment design variations and other factors
can and will cause a change in these process conditions. It is, therefore, up to the unit
operators, supervisors and the other personnel involved in the start-up and subsequent
operation of the unit to see that the unit is being operated at maximum efficiency.
The most useful tool for detecting operational difficulties is the log sheet and listed readings
as attached to this chapter. The boardman must be careful to list each reading correctly at
the appointed time. It is then important to review all of the readings to determine what and if
any changes have occurred. No changes are to be overlooked until a reason is discovered
and corrective measures, if necessary, are taken.
The outside operator should review the process equipment operation during his routine
duties and report any abnormalities (leak, noise, etc.) to the control room personnel. Proper
coordination between the boardman and the outside operators is essential for good
operation. The following section will highlight each major piece of equipment and its
operation.
10.1 METHANATOR OPERATION

The methanator R-2301 requires very little attention. The inlet and outlet temperatures
should be monitored (TI-006 and TI-007) to ensure that no temperature excursion occurs.
Samples in the inlet stream are taken with SC-2305. Sample connection SC-2316 at the
bottom of the sulphur absorbent bed on the methanator allows product sampling for sulphur
analyzes. Sample connection SC-2306 downstream Methanator Cooler E-2303 allows
sampling for CO/CO2 analyzes. Once one of the beds is saturated, sulphur or CO/CO2
breakthrough occurs and the methanator has to be reloaded.
10.2 LIQUID FEED DRIERS OPERATION

The Feed Driers (DR-2303/2304) are sized by UOP to operate 24 hours each before
requiring regeneration. The lead drier must be regenerated once its effluent contains more
than 1 wt-ppm water indicated by Moisture Analyzer (AT-001 B). The driers are operated
such that one drier is in the lead position and the other is in the lag position, or is being
regenerated. As operating experience is gained and providing a water breakthrough is not
observed, the drying periods may be extended. Typically the driers are regenerated on a
frequent enough basis to avoid moisture breakthrough of one drier. The following guidelines
can be followed to take a drier off-line, regenerate it and bring it back on-line. Reference to
P&ID's 0021-013, -012 and -029 should be made when following through this regeneration
sequence.
The control of the sequence is fully automatic by a Drier Regeneration Control System. This
system operates the process valves and associated bleeder valves. The valving of the
driers is according the double block and bleed principle. Process valves (marked with an "X"
on P&ID's) are always double. The bleeder valve (marked with a "Y") opens when the
process valves are closed to direct the fluid that is captured between the two "X" valves to
the Bleeder Knockout Drum (D-2307). When the process valves are open, the bleeder valve
is closed.
The logic control system enables each liquid feed drier to automatically sequence through
the following steps:
1. Both driers on-line in series flow, with drier DR-2303 in lead position and drier DR-2304
in lag position
2. Bypass and isolate drier DR-2303 and place drier DR-2304 in single drier mode
3. Regenerate drier DR-2303
4. Place drier DR-2303 in series flow with drier DR-2304, with drier DR-2304 in lead
position and drier DR-2303 in lag position
5. Repeat sequence for drier DR-2304
10.2.1 BOTH DRIERS ON-LINE IN SERIES FLOW, WITH DRIER DR-2303 IN LEAD POSITION
AND DRIER DR-2304 IN LAG POSITION
Assume feed is flowing through both driers, i.e., the driers are in series with drier DR-2303
first (lead position) and drier DR-2304 second (lag position). The Moisture Analyzer (AT-001
B) sample is from the outlet of drier DR-2303. At this stage: Valves XV-067, XV-066, XV-
078, XV-077, XV-055, XV-069, XV-068 and the Bleed Valves XV-059, XV-052, XV-056, XV-
080, XV-073, XV-064 and XV-083 are open and all the others are closed.
When the moisture analyzer indicates a need to regenerate or when the scheduled
regeneration time arrives, drier DR-2303 will be isolated.
10.2.2 BYPASS AND ISOLATE DRIER DR-2303 AND PLACE DRIER DR-2304 IN SINGLE
DRIER MODE
a. START FLOW TO THE DRIER DR-2304 INLET
Close Bleed Valve XV-080 and open the drier DR-2304 Inlet Valves (XV-075 and XV-
076). Open the moisture analyzer inlet valve from the drier DR-2304 effluent (XV-070)
and close the moisture analyzer sample from drier DR-2303 (XV-055).
Flow is now essentially going through only drier DR-2304, since it is the path of least
resistance.
b. BLOCK IN DRIER DR-2303
Close the Inlet Valves to drier DR-2303 (XV-066 and XV-067). Close the outlet valves on
the crossover line (XV-078 and XV-077). The Crossover Bleeder (XV-079) and Bleed
Valve XV-065 should be opened at this time to verify that the Crossover Valves (XV-078
and XV-077) are not leaking.
Now the liquid feed is only dried by the DR-2304. DR-2303 is ready to be regenerated.

a. LINE UP THE REGENERANT FLOW TO DRIER DR-2303
Close Bleed Valve XV-064 and open drier DR-2303 Regenerant Outlet Valves (XV-062
and XV-063). Close Bleed Valve XV-052 and then open drier DR-2303 Regenerant Inlet
Valves (XV-054 and XV-053).
b. START REGENERANT FLOW
Open the Regenerant Inlet Valve (XV-087) and open the Regenerant Return Valve (XV-
085).
By opening XV-089 (PID 0021-029) isomerate from DIH net overhead line starts filling up
the Regenerant Vaporizer (E-2305). The liquid isomerate is the regenerant for the driers.
From the vaporizer the flow is sent forward through the Regenerant Superheater (A-
2301) and then establish the design regenerant flow rate of 2400 kg/h with FIK-004. The
Regenerant Condenser (E-2304) and Pressure Controller (PIK-089) should also be
commissioned. The condenser outlet is routed to the isomerate product line for storage.
c. INCREASE THE REGENERANT TEMPERATURE
Start a flow of LP steam to the regenerant vaporizer by opening XV-050 and establish
the normal level in the vaporizer. Control the steam flow to the Vaporizer Unit (PIK-088).
After a stable level has been maintained in the vaporizer, the electric superheater may
be commissioned to heat up the vaporized isomerate. The vaporized regenerant from E-
2305 will be approx. 120°C. Increase the superheater outlet temperature at a rate of
70°C/h to 315°C. The control valves are accessed from the sequence program.
d. HOT SOAK THE DRIER SIEVES
Monitor the outlet temperature of the drier with TI-019. As the water is driven off of the
sieves, the temperature will gradually increase. Hold the outlet at a minimum of 288°C
for 4 hours.
e. REDUCE THE DRIER TEMPERATURE
After the 4 hour hot hold, reduce the superheater outlet temperature to 177°C and then
shutdown the heater. Continue to circulate vaporized regenerant from the vaporizer and
cool the sieve bed to about 93°C.
f. COOL THE DRIER WITH LIQUID UPFLOW
After the drier has reached the approximate temperature of the vaporizer outlet of
approx. 120°C, the sieves are further cooled with liquid regenerant. The vapor phase
cooling prevents rapid generation of vapors during the liquid phase cooldown. Shut-off
steam to the vaporizer by closing XV-050.
Open the Liquid Coolant Inlet Valve (XV-084) and the Liquid Coolant Return Valve (XV-
086). Close the Regenerant Inlet Valve (XV-087) and close the Regenerant Return
Valve (XV-085). Cool the drier sieves upflow until the outlet regenerant return
temperature (monitored with TI-019) is less than 65°C.
g. END THE COOLDOWN PERIOD
Close the Liquid Coolant Inlet Valve (XV-084) and close the Liquid Coolant Return Valve
(XV-086). Close the drier DR-2303 Regenerant Inlet Valves (XV-054 and XV-053) and
close the drier DR-2303 Regenerant Outlet Valves (XV-062 and XV-063) and open
Bleed Valves XV-052 and XV-064. Manually close and isolate the Regenerant FIK-004
control valve station. Close Isomerate Inlet Valve (XV-089).
10.2.4 PLACE DRIER DR-2303 IN SERIES FLOW WITH DRIER DR-2304, WITH DRIER DR-
2304 IN LEAD POSITION
a. LINE UP DRIER DR-2303
Close Bleeder Valve (XV-056).
Open the drier DR-2303 Outlet Valves (XV-057and XV-058).
Close the bleeder valve on the drier DR-2304 Effluent Crossover (XV-059).
Open the drier DR-2304 Effluent Crossover Valves (XV-060 and XV-061).
b. PLACE DRIER DR-2303 IN THE LAG POSITION
Close the drier DR-2304 Outlet Valves (XV-068 and XV-069) and Bleeder Valve (XV-
071) is opened. When this is done, drier DR-2304 effluent is forced through drier DR-
2303.
NOTE: The freshly regenerated drier is inventoried with isomerate product from the
cooldown, which will be sent back to the reactor section when it is placed on stream.
This material will cause a short term drop in the lead reactor delta T.
10.2.5 REPEAT SEQUENCE FOR DRIER DR-2304

The above procedure may be used to regenerate drier DR-2304 by adjusting the valve
identification nomenclature.
10.3 MAKE UP GAS DRIERS OPERATION

The Make up Gas Driers (DR-2301/2302) are sized to operate for 24 hours each before
requiring regeneration. The lead drier is to be regenerated once the effluent indicates more
than 1 ppm water on Moisture Analyzer AT-001 A. The driers are operated in series flow
such that one drier is in the lead position and the other is in the lag position, or is being
regenerated. As operating experience is gained and providing a water breakthrough is not
observed, the drying cycle periods may be extended. The manner of performing this
operation is somewhat identical to that which was done for the liquid feed driers except that
the driers are not cooled down after regeneration. Reference to P&ID's 0021-011, -012 and
-029 should be made when following through this regeneration sequence.
The same control system that operates the Feed Driers also operates the Make up Gas
Driers. The logic control system enables each make up gas drier to automatically sequence
through the following steps:
1. Both driers on-line in series flow, with drier DR-2301 in lead position and drier DR-2302
in lag position
2. Bypass and isolate drier DR-2301 and place drier DR-2302 in single drier mode
3. Depressure drier DR-2301 and liquid fill with regenerant
4. Regenerate drier DR-2301
5. Place drier DR-2301 in series flow with drier DR-2302, with drier DR-2302 in lead
position
6. Repeat sequence for regeneration of drier DR-2302
10.3.1 BOTH DRIERS ON-LINE IN SERIES FLOW, WITH DRIER DR-2301 IN LEAD POSITION
AND DRIER DR-2302 IN LAG POSITION
Assume make up gas is flowing through both driers, i.e., the driers are in series flow with drier
DR-2301 first (lead position) and drier DR-2302 second (lag position). The Moisture
Analyzer AT-001 A sample is at the outlet of drier DR-2301. At this stage, Valves XV-027,
XV-026, XV-015, XV-042, XV-043, XV-032 and XV-029 and the Bleed Valves XV-023, XV-
012, XV-020, XV-035, XV-021, XV-041 and XV-048 are open and all the others are closed.
When the moisture analyzer indicates a need to regenerate (1 ppm H2O) or when the
scheduled regeneration time arrives, drier DR-2301 will be isolated.
10.3.2 BYPASS AND ISOLATE DRIER DR-2301 AND PLACE DRIER DR-2302 IN SINGLE
DRIER MODE
a. Ensure that Bleed Valve XV-041 is closed. Open the inlet valves to drier DR-2302 (XV-
039 and XV-040). Open the Moisture Analyzer Sample Valve (XV-034). All flow is now
essentially passing through drier DR-2302, since this is the path of least resistance.
b. Close the Moisture Analyzer Valve (XV-015) at the drier DR-2301 outlet. (The analyzer
now is monitoring only the drier DR-2302 effluent.)
c. Close the Crossover Valves on the drier DR-2301 outlet (XV-042 and XV-043). Close
the Inlet Valves to drier DR-2301 (XV-027 and XV-026).
d. Open the Bleeder Valve (XV-044) on the drier DR-2301 crossover to check for leakage
and open Bleed Valve XV-028.
e. Drier DR-2301 is now completely isolated from drier DR-2302 and drier DR-2302 is in
single drier mode.
10.3.3 DEPRESSURE DRIER DR-2301 AND LIQUID FILL WITH REGENERANT

a. Slowly depressure drier DR-2301 to flare. Open the block valves, which bypass PSV-
003 at the drier outlet (XV-011 and XV-010).
b. Commission the Regenerant Condenser (E-2304) and regenerant Pressure Controller
PIK-089. Establish the design regenerant rate and liquid fill drier DR-2301 with cold
regenerant. Displace the hydrogen gas out to the flare header. Filling is complete when
liquid is observed flowing through the sight flow glass at the drier outlet.
Ensure that Bleed Valve XV-021 is closed.
Open drier DR-2301 Regenerant Outlet Valves (XV-022 and XV-047).
Open the Liquid Filling Valve (XV-049).
Open XV-089 to take isomerate product as regenerant (see P&ID 0021-029).
Establish the design flow of cold regenerant to drier DR-2301 via the Regenerant
Vaporizer (E-2305) and Superheater (A-2301).

a. Close the Relief Valve Bypass Valves at the outlet of drier DR-2301 (XV-011and XV-
010).
Ensure Bleed Valve XV-012 is closed.
Open the Regenerant Inlet Valves to drier DR-2301 (XV-014 and XV-013).
Open the Regenerant Return Valve (XV-051), P&ID 0021-012 and close the Liquid
Filling Valve (XV-049).
b. Establish the design regenerant flow rate of 2400 kg/h to the drier with FIK-004.
Commission the LP steam to the regenerant vaporizer by opening XV-050 and establish
the normal level in the vaporizer. The vaporized regenerant from E-2305 will be approx.
120°C.
At this point, there will be saturated vapors flowing to the drier, displacing the liquid
through the regenerant condenser and out to storage.
The control valves are accessed from the sequence program.
c. Start the Regenerant Superheater A-2301 and increase the regenerant temperature to
design of 315°C at a rate of 70°C per hour.
d. As the water is driven off the molecular sieves, the drier outlet temperature will gradually
increase. When the temperature (TI-008) at the drier outlet reaches 288°C, continue to
hold for a minimum of two hours.
e. At the end of the two-hour hold period, reduce the regenerant superheater outlet
temperature to about 177°C and shutdown the heater. Continue cooling with vapors until
the Drier Outlet (TI-008) reaches 204°C.
f. Discontinue steam flow to the vaporizer (close XV-050) and stop regenerant flow to drier
DR-2301 by closing XV-089 and XV-051. Block in the regenerant (FIK-004) and close
the Regenerant Inlet Valve to drier DR-2301 (XV-014). Close the Second Drier Inlet
Valve (XV-013). The Bleed Valve XV-012 can now be opened.
NOTE: If desired, regenerant circulation may be continued by circulation through the Liquid
Filling Valve (XV-049) and the Regenerant Return Valve (XV-051). XV-089 is then not
closed.
g. Isolate drier DR-2301 from the regeneration section. Close the drier DR-2301
Regenerant Outlet Valves (XV-022 and XV-047) and open Bleed Valve XV-021.
10.3.5 PLACE DRIER DR-2301 IN SERIES FLOW WITH DRIER DR-2302, WITH DRIER DR-
2302 IN LEAD POSITION AND DRIER DR-2301 IN LAG POSITION
a. Pressure up drier DR-2301. Ensure Bleed Valve XV-020 is closed. Open the Valve (XV-
019) in the outlet of the drier just downstream of the pressure-up valve. Then open the
Pressure-up Valve (XV-018). Flow is routed through a restriction orifice thereby providing
a controlled pressure-up rate.
b. Open the Outlet Valve of drier DR-2301 (XV-016) and close the Crossover Bleeder Valve
(XV-023) once drier DR-2301 is at process pressure (37.0 kg/cm² g).
c. Open the Crossover Valves from drier DR-2302 outlet to drier DR-2301 inlet (XV-024
and XV-025). Close the Pressuring Valve for drier DR-2301 (XV-018).
Most of the flow is still going only through drier DR-2302 since it provides the path of
least resistance.
d. Slowly close the drier DR-2302 Outlet Valves (XV-029 and XV-032). This forces all of the
make-up gas flow to flow through drier DR-2301 now in the lag position. The Bleed Valve
XV-031 can now be opened.
NOTE: Since drier DR-2301 contains some regenerant vapors at a relatively high
temperature, an upset in the make-up hydrogen analyzer and Fl reading will occur when
the drier is swung on line. It is possible to experience reactor and stabilizer temperature
and pressure fluctuations.
10.3.6 REPEAT SEQUENCE FOR REGENERATION OF DRIER DR-2302

The driers are in series flow operation with drier DR-2302 in the lead position and drier DR-
2301 in the lag position. When the scheduled time for drier DR-2302 regeneration occurs or
the moisture analyzer increases to 1 ppm H2O, this drier must be isolated and regenerated.
The above procedure may be used by adjusting the valve identification nomenclature for drier
DR-2302.
10.4 REACTOR OPERATIONS

The Reactor System (R-2302/2303) is typically designed to operate at a minimum pressure
of 31.6 kg/cm² g. Lead inlet temperatures range from 118°C to 162°C and lag reactor inlet
temperatures range from 98°C to 155°C.
10.4.1 PENEX REACTOR TEMPERATURES

As the catalyst ages in the first reactor it will be necessary to increase the first reactor inlet
temperature to obtain the maximum benefit from the catalyst. The temperature should be
adjusted to maximize the isomerization in the first reactor and then adjust the second
reactor inlet temperature to maintain the desired product octane number. Lower reactor
temperatures favor higher equilibrium ratios of the iso-compounds in the product.
10.4.2 LEAD REACTOR EFFLUENT SAMPLE

A lead reactor effluent sample should be obtained by condensing the sample stream at a
pressure as close as possible to the plant operating pressure. The performance of the
catalyst in the lead stage is determined by evaluating the composition and iso-ratios of this
stream (sample point connection SC-2303). This sample should be taken on a weekly basis
at a minimum to provide information on the lead reactor catalyst activity and history. This
sample will contain levels of HCI, which should be communicated to the laboratory.
10.4.3 HYDROGEN TO HYDROCARBON RATIO

For the Penex unit, the design H2/HCBN ratio is 0.05 moles hydrogen at the lag reactor
outlet per mole of charge. Operating with too low H2 circulation could result in increased
coking or flow maldistribution in the reactors. The H2/HCBN ratio is calculated by
determining the total molar flow rate of hydrogen in the caustic scrubber off gas and dividing
this by the total molar flow rate of the reactor liquid charge (computing device FFI-050). The
H2/HCBN ratio at the inlet of the reactor is also determined by computing device FFI-051. It
is the moles content H2 in the make-up gas divided by the moles content of liquid feed,
normally 0.20.
If it is determined that the H2/HCBN ratio is below 0.05, the make-up gas flow rate should be
increased to increase the ratio. Hydrogen analyzers are provided on both the make-up gas
and scrubber off gas to aid in this determination (AI-002 and AI-003).
10.5 STABILIZER OPERATION

The Stabilizer (T-2301) is designed to depropanize the isomerate. Periodic laboratory tests
should also be made to verify that essentially no chloride is exiting with the isomerate. If HCI
is found in the bottoms stream, an increase in the column reflux rate is recommended. Since
the isomerate is finally used to regenerate the driers, it is important that the regenerant is
free of HCI.
10.6 STABILIZER NET GAS SCRUBBER OPERATION

The gases from the unit containing HCI are scrubbed with a 10 wt% caustic solution in the
Net Gas Scrubber (T-2302). This is accomplished by contacting the rising acidic gases
countercurrently with caustic. The circulation rate of caustic is 7.0 m3/h for the upper section
and 3.9 m3/h for the lower section.
The caustic level in the scrubber is to be held at a point 300-600 mm below the caustic
distributor just below the packed section.
The caustic is to be changed out before it falls below 2 wt% NaOH. The temperature of the
scrubber should be maintained close to the same temperature of the stabilizer overhead
receiver in order to avoid forming a liquid hydrocarbon phase which can cause foaming and
operating problems with the scrubber.
The pH and NaOH wt% is to be checked in the circulating water. The circulating water is to
be changed out if the sodium hydroxide concentration exceeds 2 wt% NaOH or if the water
wash should ever go acidic.
10.7 DE-ISOHEXANIZER COLUMN OPERATION

The De-Isohexanizer (DIH) column (T-2303) is designed to separate dimethylbutanes and
pentanes from other C6 isomers and C7+ from the Isomerization Unit. Periodic laboratory
tests should be made to verify the C6 isomers content of the bottoms draw, the
methylpentanes content of the overhead draw and to check the composition of the sidedraw
recycle to the isomerization unit.
The reflux to feed ratio controls the fractionation efficiency for the key components in the
DIH. An increase in reflux to feed will improve efficiency until tray flooding occurs. Typically,
the reflux to feed volume ratio will range from 3.0 to 4.0. The Tray Temperature Control TIC-
047 is located on tray 5 from the top. The TIC will indirectly control the reflux to the column.
The tray temperature is directly related to the composition on the tray for a given pressure.
Increasing the tray temperature will increase the heavier methylpentanes content in the
overhead. The increase in the TIC indication will close off the product flow by FIC-031,
causing the overhead receiver level to rise, which will cause an automatic increase in the
reflux flow which is reset by the receiver level. Decreasing temperature on the TIC will
reduce top temperature and increase the C6 isomers content in the bottoms. The normal top
temperature at TI-045 is 72°C.
The TIC can be overridden by the Analyzer Calculator AY-005 B, in case either of side draw
analyzer AT-004 A/B or overhead analyzer AT-005 A/B is offspec.
Overhead product is generally sent directly to storage. Very often part of the overhead liquid
is used for drier regeneration. After service in the drier regeneration, the spent regenerant
joins the product out to storage.
Bottoms from the DIH column are sent to storage with the overhead product. The bottoms
product from the column is a small flow. It is yielded from the column on flow control.
The octane of the DIH overhead product is set by two independent variables:
a. The pentane composition of the overhead. The total amount of pentane in this stream is
set by the feedstock composition. The iso-pentane content is then set by the degree of
C5 isomerization in the reactors. For a given feedstock composition the octane of the
overhead is improved by maximizing the IC5/C5P ratio in the overhead product. Since the
pentanes in the product are processed "once through", the higher the concentration of
pentanes in the feedstock, the lower the product octane will be.
b. The amount of 2-methylpentane and 3-methylpentane in the overhead. Since these
components have an octane blending value of about 75, the higher their concentration in
the overhead product, the lower the octane will be. Since eliminating all of the
methylpentanes would require; a) more trays, b) more reflux, and c) more recycle to the
reactor section (higher Combined Feed Rate (CFR)), an economic compromise must be
made to adjust the product octane vs. utility consumption.
The key to optimizing the column is to minimize the utilities (heat input), while maximizing
the separation of the dimethylbutanes and pentanes overhead and maximizing the recovery
of the methylpentanes. It is possible to operate the column with too much heat input and
produce on spec material. The challenge to the boardman and the refinery as a whole is to
operate the column in such a fashion that just enough heat input is introduced to the column
to give the desired split. This will only be accomplished through time and operator
experience with the unit. Some DIH columns and isomerization units use a UOP online
optimizer system, which continuously adjusts isomerization reactor and DIH conditions or
changes in fresh feedstock and rates. The combined isomerization unit with DIH is a very
dynamic combination where full benefit is difficult to achieve without frequent adjustment
from input changes.
10.8 PREVENTIVE MAINTENANCE

Below are several items to remain conscious of to help ensure maximum life from the Penex
catalyst.
a. Valves on both the make-up gas and liquid feed driers should be checked, repaired and
replaced, if necessary, to insure a positive shutoff when required. Testing of valves on
both the liquid feed and make-up gas driers for leaks should be carried out at least once
per month; refer to the "Drier Manifold Valve Leak Testing Procedure" in Chapter 7 §3 of
this manual. An indication of leakage from MUG on liquid feed driers can be obtained
from FAH-006, located on the flare header line from the Bleeder Knock-Out Drum D-
2307.
b. The organic chloride injection pump should be kept in an operable state, i.e. leakage at
the plunger.
c. Consider replacement of the drier sieves after 500 cycles. The sieve vendor can verify
the condition of the sieves.
d. The moisture analyzers should be verified frequently for response and accuracy.
e. Routine analyses for feed contaminants and compositions should be performed.

10.9 TROUBLESHOOTING
Troubleshooting of a PENEX unit, like any process unit, should be an ongoing part of
normal operations. Daily logs of operations are recorded and should be reviewed to catch
any changes before they become problems. Any unexplained changes should be followed-
up on to identify their source and the necessary corrections should be made. Presented
below is a table, which attempts to guide corrective actions for problems, which are peculiar
to PENEX units. This table is a PENEX Unit Troubleshooting Guide.
Table 6.10.1 – PENEX Unit Troubleshooting Guide
Problem Possible Cause(s) Solution(s)

A Low Product 1. Feedstock composition 1a. Check iso-ratios
Octane change
1b. Optimize for new feedstock
2. High C6 paraffins in feed 2. Return to design feedstock (see

Equilibrium Octanes)
3. High C6 cyclics in feed 3. Adjust splitter operation (send 90%

C6 cyclics to reformer)
4. Low iso-ratios 4. See below
5. Cross leakage 5. Check for benzene in product
6. Contaminated feed 6. Check for sulfur/other poisons
B Low Iso- 1. High LHSV 1. Reduce feed rate to design

Ratios
2. High H2/HC ratio 2. Reduce gas rate to design
3. High benzene in feed 3a. Return to design feedstock

3b. Adjust reactor temperature to
compensate for high delta T
3c. Reduce LHSV
4. High C7+ in feed 4. Adjust splitter operation
5. High C6 cyclics in feed 5a. Adjust splitter operation (send 90%

of the cyclohexane to the reformer)
5b. Increase the lead reactor
temperature to optimize C6 ring
opening
6. Reactor temperatures 6. Optimize reactor temperatures
either too high or too low
7. Sulfur in liquid feed 7a. Correct NHT operations

7b. Check for combined feed exchanger
leaks in the NHT
7c. Correct stripper operations
7d. Has feedstock source changed on
the NHT?

B Low Iso-Ratios 8. H2S in make-up hydrogen 8a. Correct desulfurizer operations
(continued)
8b. Check for exchanger leaks
8c. Remove H2S from reformer recycle gas
8d. Check for benzene in reactor effluent

8e. Check for H2S in stabilizer gas
9. H2O in liquid feed or make- 9a. Correct drier operations and

up hydrogen regenerations
9b. See problem: H2O breakthrough from
driers
9c. Purge equipment to remove air and
water after maintenance before placing
on line
9d. Bypass reactors until problem is solved
10. Erratic feed flow rates 10a. Stabilize feed flow and optimize reactor
temperatures
10b. Check feed surge drum pressure
controller
10c. Check pump suction strainer
10d. Check naphtha splitter operation
11. Deactivated or dead 11a. Check inter reactor sample

catalyst
11b. Determine type and source of catalyst
poison
11c. Perform sulfur strip if warranted
11d. Replace catalyst
12. Inaccurate lab results 12a. Correct sampling procedure

12b. Troubleshoot lab equipment
12c. Verify lab is using correct test method
13. Faulty thermocouples 13. Correct thermocouple and optimize

reactor temperatures
14. Poor drier regeneration 14. See problem: H2O breakthrough from
driers
15. Feed contamination 15a. Identify type of contaminant and

eliminate
15b. See Chapter 12, Table 2: PENEX
Streams Contamination Limits ane
Performance Identifiers
16. Reactor channeling 16a. Check proper reactor internals installed
correctly
16b. Check dense loading results

C H2O 1. Channeling - upset 1. Check and reload driers sieves
Breakthrough
from Driers 2. HCI in stabilizer bottoms 2. Correct stabilizer operations (verify
poisoning mol sieves during reflux at design)
regeneration
3. Insufficient 3a. Regenerate driers more often
regeneration frequency
3b. Calibrate moisture analyzers
4. Sieves contaminated with 4a. Identify and eliminate source of heavy

heavy oil oil
4b Replace drier sieves
4c. Check lube oil mist eliminator
performance
5. Inaccurate moisture 5. Troubleshoot moisture analyzer.
analyzer Replace probe
6. Spent drier sieves 6a. Replace sieves after 500 regenerations

6b. Have sieves activity checked
7. Leaking valves 7. Use double blocks and bleeds correctly.

Repair seats
8. Excessively long 8. See problem: Long drier regeneration

regeneration cycle cycle
9. High drier temperatures 9. Check cooler on liquid feed or make-up

gas
D Long Drier 1. Low regeneration bed 1a. Identify and replace leaking valves
Regeneration temperature
1b. Check regeneration flow data and
Cycle
pressure. Correct to design
1c. Check vaporizer and superheater
1d. Check thermocouples
1e. Check insulation
1f. Use double block and bleeds correctly
2. Superheater tripping out 2a. Check superheater element

2b. Check fuse
2c. Check regeneration flow rate, return to
design
3. Vaporizer flooding 3a. Check vaporizer level controller

3b. Return to design flow rate and pressure
3c. Check steam trap
3d. Check steam pressure

E Reactor 1. Regenerated liquid drier put 1. No problem - temperatures will return to
Temperatures on line normal within one hour
(or delta T's)
Decrease 2. H2O breakthrough from 2a. See problem: H2O breakthrough from
driers driers
2b. Bypass reactors and regenerate driers
3. Sulfur or H2S breakthrough 3a. Bypass reactors

from driers
3b. Determine and eliminate source of high
sulfur or H2S
3c. Regenerate driers
3d. Check for H2S in recycle gas and in
stabilizer off-gas
4. Feed composition changes 4a. Correct splitter operations

4b. Optimize for new feedstock
5. Feed contamination 5a. Identify type of contaminate and

eliminate
5b. See Chapter 12, Table 2: PENEX
Streams Contamination Limits ane
Performance Identifiers
6. Increase feed rate 6a. Stabilize operations at new feed rate
6b. Check H2/HC ratio
7. Charge heater upset (loss of 7. Check charge heater

heating medium)
8. Loss of organic chloride 8a. Check organic chloride injection

injection package
8b. Inject only UOP approved organic
chloride compounds
F Benzene in 1. HCFX leak 1. Fix leak

Lead Reactor
Effluent 2. Sulfur attenuation of catalyst 2. Identify source of sulfur and eliminate
3. Carbon oxide attenuation of 3. Remove source of carbon oxides

catalyst
4. Incorrect lab analysis 4. Recheck result
G Benzene in 1. CCFX leak 1. Fix leak

Tail Reactor
Effluent 2. Sulfur attenuation of 2a. Identify source of sulfur and eliminate
catalyst
2b. Perform sulfur strip
3. Carbon oxide attenuation of 3. Remove source of carbon oxides

catalyst

H High 1. Exchanger fouling 1a. Correct cooling water problems
Temperatures
1b. Clean exchanger
Out of Water
Coolers
I Chlorides in 1. Poor stabilizer operation 1. Correct stabilizer operation. Verify R/F
Product is at design or higher
2. Stabilizer feed/effluent 2. Fix leak

exchanger leak
J Chlorides in 1. Weak caustic 1. Charge-out spent caustic when 2 wt%

Product NaOH. Make-up fresh 14.4 wt% NaOH
Scrubber Off-
gas 2. Inadequate caustic 2a. Clean pump suction strainer(s)
circulation
2b. Return to design circulation rate
3. Erratic gas flow 3. Check stabilizer and scrubber pressure

controllers
4. Caustic level being held too 4. Hold level up in packed section.

low Calibrate level indicators
5. Contaminated sample lines 5. Use clean sample lines for detector tube
connection
K Hydrocarbon 1. Caustic temperature below 1. Check stabilizer overhead temperature.

Layer on stabilizer off-gas Return to design
Caustic in temperature
Scrubber
2. Poor stabilizer operations 2. Correct stabilizer operations. Return
(heavy ends in overhead) reflux rate to design
L High RVP in 1. Poor stabilizer operation 1. Correct stabilizer operation: establish

Product design reflux and overhead temperature
2. Butanes in feedstock 2. Verify feedstock is normal per GLC on

feed
M Caustic 1. Dirty make-up caustic 1. Use only fresh, clean caustic

Circulation
Pumps 2. High wt% NaOH 2a. Dilute caustic to 10 wt% NaOH
Plugging
2b. Correct condensate injection rate

N Caustic Carry- 1. Erratic gas flow rate 1. Correct pressure controllers on
over from stabilizer and scrubber
Scrubber
2. Scrubber plugged due 2a. Dilute caustic to 10wt%
to too strong or fouled
2b. Use only fresh, clean caustic for make-
caustic
up
2c. Replace rings in packed section
2d. Shutdown to clean vessel
3. Foaming 3. Contaminated caustic, liquid

hydrocarbon layer
O Corrosion in 1. Too high caustic 1a. Limit caustic strength to 10 wt%

Scrubber temperature
1 b. Do not steam out scrubber at shutdown
2. Dry areas in scrubber 2a. If caustic level is kept in packed area,
use the lower caustic spray nozzle
during caustic change-out
2b. If caustic level is kept below packed
area, maintain lower spray ring flow
continuously
3. Improper caustic 3a. 2 wt% min NaOH at change-out
change-out procedure
3b. Regularly scheduled change-out
3c. Do not use pH as control, use caustic
strength as wt% NaOH
P Corrosion in 1. Chlorides in regenerant 1. Correct stabilizer operation. Verify R/F

Regeneration is at design or higher
Gas Cooler
2. Stabilizer feed/effluent 2. Fix leak
exchanger leak causing
chlorides in regenerant
3. HCl in make-up gas 3. Eliminate HCl
4. Moisture build-up from 4. Minimum regeneration cycle of 1 regen

insufficient drier per drier per week (i.e. 4 regenerations
regenerations and HCl per week)
present

Q Sulfur in 1. Combined feed exchanger 1. Repair leaks.
Liquid Feed leaks in the NHT
2. Poor stripper operations 2. Correct stripper operations. Establish a

RIF of about 0.3
3. Start-up bypass valves 3. Blind-off all unnecessary lines and

leaking check double blocks and bleeds
4. Contaminated gas blanket 4a. Use only dry make-up hydrogen for gas
on feed surge drum blanket
4b. Check for H2S breakthrough around
make-up hydrogen driers
R Oxygenates in 1. Feed coming from storage 1. Use only fresh feed. Route storage back
Liquid Feed through desulfurizer
2. Feed blanketed with fuel or 2. Do not blanket liquid feed with CO/CO2
natural gas containing gases
S Insufficient 1. Low reformer feed rates or 1. Reduce PENEX feed rate until reformer
Make-up temperatures back up to normal
Hydrogen
T CO/CO2 in 1. Poor methanator operations 1. Correct methanator operation to remove

Make-up all CO. Check bypass
Hydrogen
2. Drier needs regeneration 2. Regenerate drier to monitor for CO2
breakthrough
3. Cyclic reforming operations 3. Methanator required to remove CO;

additional mol sieves to remove CO2 or
PSA needed
4. High moisture content in 4a. Check water oxygenate content of CCR
CCR platforming unit platforming feed
recycle gas
4b. Check water content of CCR
regeneration air. Possible spent drier
5. Poor PSA operations 5. Adjust PSA to reject carbon oxides
6. Cross-contamination in 6. Blind contaminated sources from

hydrogen header PENEX make-up gas
10.10 TYPICAL EXAMPLE FOR COLLECTING DATA & QUALITY CONTROL

To assist the personnel which is operating the Penex/DIH Process Unit, the following table
summarizes the main parameters (flows, temperatures, pressures, etc.) required for a good
monitoring of the operation.
This table, to be used as a logsheet, indicates for each parameter:
♦ the measurement tag number,
♦ its description,
♦ the normal (100% feed stock rate) and the turndown (50% feed stock rate) expected
values
CHAPTER 7
NORMAL SHUTDOWN
CONTENTS

1.1 GENERAL
1.2 TOTAL UNIT SHUTDOWN
1.3 PARTIAL UNIT SHUTDOWN
1.4 METHANATOR SHUTDOWN
1.5 SHUTDOWN PRECAUTIONS
1.5.1 BACKGROUND ON NICKEL CARBONYL
2. CATALYST UNLOADING AND HANDLING PROCEDURE

2.1 I-8 PLUS/I-82 CATALYSTS UNLOADING AND HANDLING
2.1.1 PREPARATION FOR UNLOADING
2.1.2 I-8 PLUS/I-82 CATALYSTS UNLOADING AND HANDLING
2.2 ADS-11 UNLOADING AND HANDLING

2.3 METHANATOR CATALYSTS UNLOADING AND HANDLING
2.4 DRIER UNLOADING
3.1 DRIER MANIFOLD VALVE LEAK TESTING PROCEDURE
3.2 SULFUR STRIPPING

3.3 METHANATOR TEMPERATURE EXCURSION
1.1 GENERAL
A normal shutdown is one, which is planned in advance for the purpose of scheduled
maintenance or repairs to equipment. The scope of maintenance work will, in some
degree, determine the extent of plant conditioning required to gain access to the
necessary equipment. For instance, in a short duration shutdown it may not be
necessary to gas-free and inert the entire unit if access is only required to certain pieces
of equipment which can be safely isolated. The main objectives of the normal shutdown
procedures are therefore:
♦ To stop production in the unit in a safe and efficient manner.
♦ To give guidelines, in a generalized manner, on preparation of the unit for
maintenance activities.
In a planned shutdown, review all records to determine what inspections and repair work
must be accomplished during the shutdown. Prepare a shutdown schedule including
plans for pre-arranging feed and product storage tank inventories to conserve turnaround
time. Notify all collateral activities of the shutdown schedule so that all phases can be
properly coordinated. Arrange for all required parts, tools and services in advance.
Arrange for close liaison with affected operating units to minimize or eliminate operating
penalties.
When shutting down, steps should be taken to prevent catalyst (to upstream units),
adsorbent, equipment damage from expansion, contraction and thermal shock or
unusual pressure or vacuum, etc. Arrange for the continued availability of utilities and
purge gases for as long as required. Purge with care all vessels, using steam for those
that are not subject to condensation damage, and inert gas for the critical vessels until all
equipment is free of hydrocarbon liquids and gases. Steam should not be allowed to
contact the catalyst or adsorbent. Avoid the formation of a vacuum that could cause
vessel collapse if insufficient inert gas is admitted following condensation or draining.
Ventilate thoroughly and check the vessel atmosphere before entering or starting repairs.
Rigorously observe all safety precautions, using special care to avoid loss of
hydrocarbon liquids directly to the sewer. Always assume equipment contains hot
hydrocarbon liquids or vapors under pressure until proven otherwise.
1.2 TOTAL UNIT SHUTDOWN

If the entire unit is to be shutdown for an extended period, the following procedure can
be used:
1. Make provisions to take care of temporarily produced off-spec product.
2. Discontinue all drier regenerations at a point where the drier being regenerated has
just completed its regeneration cycle.
3. Increase the make-up gas flow to the maximum possible.
4. Reduce the reactor (R-2302/2303) inlet temperatures to 121°C (TIC-056 and TIC-
024) at a rate of 28°C per hour. Leave the charge rate constant since a sharp
reduction could result in high reactor severity and a temperature excursion.
5. When the reactor temperatures reach 121°C, decrease the charge rate slowly to 50%
of design. Reduce the charge in increments of 5% of scale every 15 minutes.
Continue to sweep the reactor with at least a design flow of make-up gas. Maintain
the reactor temperatures at 121°C.
6. After the charge rate has been reduced, depressure the reactor circuit with PV-097 to
21 kg/cm² g. Depressure at a rate which allows stabilizer pressure control.
7. Cool the reactors to 93°C and stabilize the temperature. When the reactor
temperature reach approx. 105°C, stop the chloride injection. Maintain these
conditions for one hour after the chloride injection has been stopped, in order to
sweep chloride from the feed circuit upstream of the reactors, then proceed to step 8.
8. Bypass the reactor feed to the Stabilizer (T-2301). Open block valves at 4”-PZ-
230130. During the period charge is cut out, try to minimize low flow of liquid over the
catalyst, i.e. cut the feed out as quickly as possible. Close block valves at 6”-PZ-
230126.
9. Sweep the reactor circuit with the design flow of hydrogen until the temperatures are
65°C. Stop the hydrogen flow when the reactors have cooled.
10. Maintain pressure on the reactors and ensure that they are fully isolated. The reactor
circuit pressure should be kept positive to avoid ingress of contaminants. As the
reactor cools, there is a risk of developing a vacuum on the system, which could
result in air ingress. Block in steam heaters and water coolers as they are taken out of
service and drain the waterside.
11. If the shutdown is going to be short in duration, the Stabilizer (T-2301) and De-
isohexanizer (T-2303) can be left in operation. If not, the stabilizer and de-isohexanizer
should be shutdown in an orderly manner.
12. If the stabilizer and de-isohexanizer are to be shutdown, be careful to avoid
depressuring the stabilizer below the scrubber pressure. There is a risk, if the check
valve in the stabilizer off-gas line does not hold, of backing up caustic from the Net
Gas Scrubber (T-2302) to the stabilizer. When the stabilizer has been shutdown,
block in the off-gas line to the scrubber at 3”-PG-230183.
13. Gradually begin to reduce heat input to the reboilers. As the columns cool and
overhead reflux decreases, shutdown the Reflux Pumps (P-2304 A/B and P-2312
A/B). Turn them on briefly to reduce any level build up in the Overhead Receiver (D-
2303 and D-2306). Once the columns collapse and Reboiler (E-2309 and E-2316)
temperatures are close to the feed inlet, cut charge going to the columns.
14. If the columns are being shutdown in conjunction with maintenance on upstream units
and do not need to be opened up, leave suitable levels in reboilers and receivers to
help during the restart of the columns. Leave pressure on the columns since cooling
vapors can create a vacuum condition. If the columns need to be opened, de-
inventory the reboilers and receivers. Follow refinery standard steam out procedures.
15. Depending upon the extent and the reason for the shutdown, the following will apply:
♦ If any equipment or vessel upstream and downstream of the reactor circuit is to be
opened, it is to be properly purged with nitrogen. If personnel entry to this equipment
is then to be made, it must be prepared for entry by purging it with air (after N2 purge)
followed by a check by the refinery safety department.
♦ If any equipment or vessels in the reactor circuit (excluding the reactors) are to be
opened, they are to be properly purged with nitrogen. If personnel entry to this
equipment is then to be made, it must be prepared for entry by purging it with air
(after N2 purge) followed by a check by the refinery safety department. If the work
(whatever it may be) is extensive in this area, it may be necessary to re-acidize the
entire reactor circuit with anhydrous HCl as outlined in this initial start-up procedures.
♦ If the reactors are to be unloaded, refer to catalyst unloading § 2.
♦ If the stabilizer is to be opened for inspection, the tower should be operated for a
period of time on feed which is bypassing the reactor. A purge of make-up gas should
be sent to the tower to help purge HCl from the overhead. After there is no
measurable HCl in the overhead, the tower may be shutdown and purged of
hydrocarbon per normal refinery procedure.
1.3 PARTIAL UNIT SHUTDOWN

In the event it becomes necessary to change the catalyst in one reactor, carry out the
steps detailed in § 1.2 through step 6, then follow the steps below:
1. Open the make-up gas purge line to the reactor to be taken off line. Maintain the
purge gas flow at the design value. Controlled by globe valve at 1½”-PG-230154 and
flow indicated at FI-015.
2. Begin admitting Charge Heater (E-2308) outlet material into the Reactor (R-
2302/2303) to be left on stream and block in the feed to the reactor to be replaced.
3. After purging the lead reactor for at least 4 hours, temporarily stop the purge. Block in
the valve in the return line from Hot Combined Feed Exchanger (E-2307 A/B) to the
reactor to be left on stream and immediately open the single reactor bypass 6”-PZ-
230140. Immediately re-establish the hydrogen purge.
4. Open the valve on the outlet of the reactor to be left on stream to the hot combined
feed exchanger.
5. Close the valve on the outlet from the reactor to be left on stream to the Cold
Combined Feed Exchanger (E-2306). Process flow will now be from the combined
feed charge heater through the reactor left on stream, through the hot combined feed
exchanger and on into the cold combined feed exchanger.
6. Open the valve in the outlet from the reactor to be replaced to the cold combined feed
exchanger and close the outlet valve from this reactor to the hot combined feed
exchanger.
7. Continue to purge the reactor to be unloaded. This reactor should be purged for a
period of time long enough to remove hydrocarbon from the reactor and to cool the
catalyst bed below 65°C. Increase reactor pressure back up to the design normal
operating pressure, 31.7 kg/cm² g at PIC-097.
8. Block in the gas purge to the reactor to be replaced, block in the outlet valve of the
reactor being replaced going to the cold combined feed exchanger and then depressure
the reactor to the flare. Increase the reactor circuit pressure back to design.
9. Evacuate the reactor three times to about 600 mm Hg, breaking the vacuum with dry
nitrogen to 0.35 kg/cm² g each time. Purge the reactor to the flare with nitrogen for an
hour after breaking each vacuum.
10.With a small nitrogen purge on the reactor, insert spectacle blinds at the inlet and
outlet of the reactors and proceed to unload the catalyst as outlined in the following §
2.1 of this chapter.
1.4 METHANATOR SHUTDOWN

If the shutdown is temporary and expected to last less than 2 hours:
1. As soon as there is no more hydrogen demand in the Isomerization Unit, put makeup
gas inlet valve 012-FV-013 on manual control and fix valve set point to keep minimum N2
flow through methanator system.
2. Open the vent to the flare and keep the hydrogen flow to a minimum.
3. Lower the reactor inlet temperature to 204°C and maintain this temperature until there is
a demand for hydrogen in the Isomerization unit.
If the shutdown will be more than just a few hours:
4. Stop makeup gas flow and depressure the methanator system through the vent to the
flare while maintaining a 204°C reactor inlet temperature. Depressure to 1.5 kg/cm² less
than the nitrogen header pressure.
5. Introduce nitrogen to the methanator by opening valve on line 1”-N-230011 and cool
down to 66°C at the reactor outlet by cutting out the heating medium to the charge
heater E-2308 and purging nitrogen through the reactor to the flare.
6. At a reactor outlet temperature of 66°C, block in the vent to the flare and the nitrogen
source and maintain under nitrogen pressure.
1.5 SHUTDOWN PRECAUTIONS
1.5.1 BACKGROUND ON NICKEL CARBONYL

In Process units such as naphtha hydrotreating units and methanator, the potential for
forming nickel carbonyl exists only with the catalysts and adsorbents containing nickel
(Puraspec 2443) and only during regeneration or during the handling of unregenerated
catalyst. Care must be used to ensure that the procedures used will prevent the
formation of nickel carbonyl. Data has been published showing the equilibrium
concentration of Ni(CO)4 versus temperature, pressure and CO concentration in a gas.
The nickel carbonyl concentration drops rapidly with increasing temperature and
decreasing CO concentration. At 7 kg/cm2g with 0.5 mol% CO in the gas, the nickel
carbonyl concentration is at the maximum recommended spot level of 0.04 ppm at 149°C
and 0.001 ppm at 182°C.
The following practices should be followed to prevent the formation of nickel carbonyl:
1. Once a reactor containing a nickel catalyst has been exposed to oxidizing conditions
(regeneration), a measurable concentration of oxygen must be maintained until the
combustion of all carbon ceases and all CO2 has been purged from the system.
2. Once a reactor containing a nickel catalyst is in a reducing atmosphere and
regeneration is not desirable, maintain the system in a reducing or inert atmosphere until
all the catalyst has been cooled to at least 65°C. Unregenerated catalyst should be
unloaded with both the vessel and drum N2 purged before receiving used catalyst.
Oxidation (burning) must be avoided.
These are many published techniques for determining the concentration of nickel carbonyl
in air (such as a vessel to be entered for maintenance) and several direct reading
instruments are available commercially. For further information, see:
American Industrial Hygiene Assoc. Journal
May-June, 1968
January-February, 1965
2. CATALYST UNLOADING AND HANDLING PROCEDURE
2.1 I-8 PLUS/I-82 CATALYSTS UNLOADING AND HANDLING
2.1.1 PREPARATION FOR UNLOADING

When it is determined that the catalyst in the lead reactor has been completely deactivated,
the catalyst may be changed out while maintaining the lag reactor in service. Single
reactor operation is established by starting flow to the inlet of the "lag" reactor and
blocking in flow at the "lead" reactor inlet. The hydrocarbons are purged from the
deactivated reactor by establishing H2 purge gas flow through the reactor purging out to
the reactor effluent section. The reactor is then evacuated and purged with nitrogen. The
"Partial Unit Shutdown Procedure" in this chapter should be followed to shutdown the lead
reactor for catalyst changeout.
2.1.2 I-8 PLUS/I-82 CATALYSTS UNLOADING AND HANDLING

The same precautions used to keep air away from fresh catalyst must be used when
unloading spent catalyst from a reactor. Spent catalyst contains a large amount of
chloride, and any moisture that contacts the catalyst will make the material very
corrosive. At all times during the opening of the reactor and unloading of the catalyst, a
dry nitrogen gas blanket of 1.0 to 1.5 inches of water should be maintained on the
reactor. With the reactor to be replaced, taken off line and prepared as previously
outlined, the following procedure can be followed:
1. Remove the blind flange on the catalyst withdrawal nozzle and attach the catalyst
unloading spout.
2. The spent catalyst must be loaded into the original catalyst drums and plastic liners to
protect against corrosion during shipment. During the catalyst run, the drums should
be stored in a dry location and protected from damage. Detailed unloading steps are
outlined below:
a. Place an empty catalyst drum on a scale, then put the inner plastic catalyst bag
with the unloading neck inside the outer heavy plastic bag. N2 purge the inner bag.
b. Slip the plastic unloading neck over the catalyst unloading spout, then remove the
catalyst support plate from the withdrawal nozzle.
c. Load approx. 115 kg of catalyst into each drum. A minor modification to the
catalyst unloading spout will allow the catalyst flow to be regulated and stopped
easily (refer to Figure 2.1).
d. When a drum is full, wire clamp the plastic unloading neck in two places, then
clamp the heavy catalyst bag around the inner bag. Close the drum tightly using
the original lids and retaining rings.
e. Take samples of the spent top, middle and bottom I-8 Plus/I-82 catalysts and send
to UOP for analyses and comments.
3. There is no need to screen the catalyst prior to returning it for platinum recovery,
since it will be screened prior to processing. However, the ceramic holddown material
will result in increased shipping costs if the catalyst is not screened. The catalyst
unloading spout could be modified to insert specially fabricated or purchased
screening equipment (refer to Figure 2.2). The holddown material that is collected
should then be manually screened a second time and any catalyst or fines that are
collected should be added to one of the drums.
4. During the unloading of the catalyst, the top manway of the reactor can be opened in
preparation for the loading of fresh catalyst. As the manway is opened, tightly cover
the open flanges with plastic. The manway and distributor should be wrapped in
plastic to protect it from moisture. The reactor manway should be tightly covered with
plastic or the catalyst loading assembly installed to conserve nitrogen during the
unloading.
5. A small amount of spent catalyst will be left in the bottom of the reactor, because the
support material is leveled and is not sloped towards the withdrawal nozzle. This
catalyst can be removed by using a very long handled, flat, shovel to "sweep" the
catalyst towards the withdrawal spout.
6. Once all spent catalyst has been removed, the catalyst support plate should be
installed, along with a coiled layer of ½” diameter ceramic fiber rope on top of the
plate in the withdrawal nozzle. The unloading spout should be removed. Replace the
gasket on the withdrawal nozzle flange and close the withdrawal nozzle. The
withdrawal sleeve can be filled with the appropriate sized support material from the
top of the reactor by using a long piece of 1½” pipe or plastic tubing and a funnel to
channel the material into the sleeve.
7. Fresh catalyst can then be loaded using the procedures outlined in Section 6.5.
NOTE: The above procedure is based on the unit being shutdown for a catalyst
change in one reactor only with the unit being kept in operation with the second
reactor set or being kept under a positive hydrogen pressure. If the unit has been
completely shutdown and equipment in the reactor section exposed to air and
moisture, the reactor circuit must be dried (including HCl addition) before the unit is
placed back on stream. If the reactor was opened to the air during the unloading, it
must be included in the drying circuit before fresh catalyst is loaded.
8. Using the above procedure, it is not necessary for a person to enter the reactor to
finish the unloading. If for any reason it becomes necessary for a person to enter the
reactor, only persons trained for inert entry taking suitable safety precautions may
enter. Safety precautions include use of a fresh air mask, safety harness, and lifeline
for a person to enter a nitrogen atmosphere.
9. Catalyst spillage should be minimized using the above procedure and the specified
unloading equipment. However, the concrete pad at the base of the reactors should
be cleaned prior to the unloading operation so that any spilled catalyst can be swept
up and placed in one of the drums.
10. The weight of catalyst unloaded should be recorded as a check on possible loss
during shipment. When the catalyst is returned for platinum recovery, it is screened to
remove oversized particles and fines (particles smaller than 14 mesh). The platinum
content of the catalyst and the fines are determined separately. As a general rule,
fines will contain approximately 20% catalyst.
11. The difference between the catalyst loaded and unloaded should be noted for
bookkeeping charges for catalyst losses.
2.2 METHANATOR CATALYSTS UNLOADING AND HANDLING

Spent catalyst is in the reduced state and it must be unloaded cool under an inert
atmosphere since contact with oxygen may result in combustion and/or the formation of
nickel carbonyl. Nickel carbonyl is extremely toxic and is dangerous at parts per billion
levels so precautions taken to exclude air must be thorough. Fire extinguishers and
steam hoses or water should be available for immediate use.
1. Isolate the cooled reactor (66°C) by blinding the inlet and outlet lines. Maintain the
nitrogen purge (if possible) and in any case, the nitrogen blanket must be maintained.
2. Monitor the methanator bed thermocouples on a routine basis and record. The board
operator must notify the field operator of any temperature increase. The use of a
portable potentiometer may also be used. A temperature increase could indicate air
entry to the catalyst bed that could possibly initiate the formation of nickel carbonyl.
3. Non-essential personnel should not be permitted in the area while the catalyst is
being dumped.
4. Personnel involved in handling spent catalyst or those working near the unloading
operations must wear full protective clothing and self-contained or air supplied
respiratory equipment.
5. Attach a nitrogen line to the top of the reactor. There should be a valve or a regulator
on the line so that the nitrogen purge can be controlled.
6. Remove the unloading nozzle blind flange and replace it with a short pipe that has a
slide valve in it. The slide valve should have a large enough opening so that the key
can be pulled through it.
7. A screening device catalyst should be empty into a drum that is being purged with
nitrogen.
8. The next drum to be filled should also be purged with nitrogen.
9. Ground the drum being filled.
10. Put the tops on the drums immediately.
11. When the reactor has been emptied, the reactor top manway can be opened and the
hold down grating removed. This work should be done while wearing self-contained
air supply safety equipment.
12. Have the refinery safety department check the unloading area and if their review
indicates no safety hazards present, then discontinue the use of the air supplied
equipment.
13. Clearly identify all drums containing the used unregenerated methanator catalyst. The
identification of these drums should include a note of caution relating to the nickel
contents of the drum.
If it is desired to oxidize the methanator catalyst prior to dumping, the following
guidelines can be followed:
1. Use nitrogen to purge the isolated methanator reactor circuit of all hydrocarbons. The
refinery Safety Department should verify this has been accomplished.
2. Maintain the methanator reactor inlet is at 149-177°C.
3. Maintain a nitrogen purge of the methanator venting to a safe location (not to flare as
oxygen may enter this system later in the procedure).
4. Introduce a small quantity of air to give 0.6 mol percent oxygen in the nitrogen
passing through the methanator. The oxygen will oxidize the methanator catalyst.
Also a temperature rise will be encountered in the catalyst bed due to this oxidation.
Do not permit the bed temperatures to exceed 400°C or the temperature limits of the
equipment, whichever is lesser. If the temperature starts to become excessive,
reduce the air rate to the methanator.
5. When the bed temperatures start to decrease, this will indicate that the oxidation has
been completed. Cool down the reactor with the nitrogen/oxygen gas mix.
Depressure the system.
6. Follow the methanator catalyst dumping procedures as outlined in the previous
unloading guidelines.
2.3 DRIER UNLOADING

Adsorbents or molecular sieves exposed to a gas or liquid stream can pick up various
materials. Trace materials can be concentrated. Some may be toxic, flammable, or
explosive, or, when exposed to air, may heat up or become poisonous. Grounding of
equipment is recommended, however, static sparks might still occur, for example, when
dumping molecular sieves from non-conducting containers or when a person removes outer
garments in low-humidity conditions. It is very important that you install appropriate blind
flanges and properly remove any potentially hazardous materials from the molecular sieves,
vessel interiors, and connected piping. Do so before you open the vessel, piping or valve
bodies to the atmosphere done by gas purging as discussed below.
The driers are typically unloaded through the manway on the side near the bottom of the
vessels. A steel unloading chute is usually attached to the manway to direct the molecular
sieve into unloading hoppers or drums. The molecular sieve may also be unloaded by
vacuuming via the top manway prior to unloading. The support balls located at the bottom of
the drier usually do not require replacement or reloading unless there has been a problem
with sieve containment or pressure drop.
The following guidelines are provided for drier unloading. Additional unloading details should
be obtained from the supplier of the adsorbents in the driers.
a. Prior to unloading the liquid feed driers it is recommended that a partial regeneration is
conducted. This step removes benzene from the molecular sieve and helps
hydrocarbon free the sieve by heating it prior to purging with nitrogen. The partial
regeneration should include the normal regeneration steps, up to the hold step at
288°C, to displace and remove benzene. Once the sieve bed has been heated, the
drier should be isolated and depressured. A nitrogen purge to flare should follow for
removing the hydrocarbons from the sieve. Occasionally, pressurize and depressurize
the vessel to ensure more complete purging. The makeup gas driers may be
evacuated and purged to aid in hydrocarbon freeing the vessels.
b. Continue to purge until the outlet nitrogen mixture is 50% below the lower explosive
limit and free of toxic materials. Then, shut off the nitrogen purge and the flare line.
c. Maintain a nitrogen blanket on the top of the vessel during unloading.
Always assume that some hazardous materials remain on the molecular sieve.
Therefore, do not enter the vessel while the molecular sieve remains inside. Toxic
fumes may be released during dumping. Always keep self-contained breathing
apparatus and fire hoses available.
If at any time during unloading, materials on the molecular sieve start to burn or to react
(give off large amounts of heat) cease dumping. Clear personnel from the area.
Properly trained personnel with self-contained breathing apparatus can then return to
stop the reaction or put out the fire. To stop the reaction, or put out the fire, use water
from fire hoses to flood the molecular sieve outside the vessel.
As with fresh molecular sieve, used molecular sieve should not be put into the mouth or
allowed to touch the eyes or skin. Workers dumping the molecular sieve should wear
gloves, eye protection, dust masks, safety shoes, and clothing that covers the body.
d. Normally, there is a stainless steel screen on top of the molecular sieve bed. Inert balls
lie on top of the screen. To make dumping easier, secure the screen to the top of the
vessel. You can do this without entering the vessel and secure the screen using a
harpoon-type tool.
e. For unloading, open the dump port and allow the molecular sieve to flow out. Once the
molecular sieve no longer flows out freely, remove the remaining portion using a rake,
hoe, shovel or a vacuum truck. Never enter the vessel to remove the remaining
molecular sieve.
f. When you discard the used molecular sieve, make sure that you discard it in an
environmentally acceptable manner. Comply fully with Federal, state and local
regulations.
g. Once you have removed all the molecular sieve, prepare the atmosphere in the vessel
for safe entry. Remove the nitrogen purge line if used and attach an air mover so that
air is expelled out of the bottom of the vessel below the bed support. The air will carry
any remaining vapors out of the vessel and away from the workers. Such vapors may
be released by molecular sieve trapped under the bed support. Leave the air mover on
at all times. Never use a plant air supply to purge the vessel with air – a plant supply
could become contaminated or be hooked up to another source by mistake.
h. After safety personnel have determined that the atmosphere inside the vessel is safe to
breathe, and is not over 10% of the lower explosive limit (LEL), a properly equipped
and trained worker may enter the vessel to inspect the bed support. Before entry, the
worker must be attached to a safety rope. Two properly trained and equipped co-
workers standing outside the entry port should constantly observe the worker in the
vessel. The co-workers should use the safety rope to prevent falls from the ladder used
to enter or leave the vessel. Also, if disabled, the worker can be removed using the
rope.
Figure 2.1
Figure 2.2
3.1 DRIER MANIFOLD VALVE LEAK TESTING PROCEDURE

Testing of valves on both liquid feed and make-up gas driers should be carried out at least
once per month, with the driers lined up in A → B series and B → A series.
The following steps should be carried out:

1. Wait until the driers are in either A → B or B → A line up.
2. Provide a water hose to wash away liquid hydrocarbons to sewer.
3. Ensure that lines on which valves are to be checked are not in use, and that both
valves of the double block are in the fully closed position.
4. Slowly open the bleeder valve and allow any liquid to drain to the Bleeder Knockout
Drum D-2307. Initially there will be a good flow, as the liquid which has accumulated
in the space, flows out (refer to figures below). After a short time, the flow should
decrease or stop completely. It is the leak after this time that should be measured.
5. Try to estimate the leak rate in cc/minute using the level gauge of the Bleeder
Knockout Drum D-2307. Note the rate, along with any other observations, on the
Leak Survey Report Sheets.
6. Once the leak has been estimated, close off the bleeder valve (except the cross-over
bleeder valves, XV-059 and XV-079, which must be left open when the cross-over is
not in use).
7. Repeat Steps 3 through 6 on as many of the lines as possible with the existing drier
line up.
8. Wait until the next time that the drier line up order is reversed and repeat Steps 1
through 6.

1. Wait until the driers are in either A→B or B→A line up.
2. Provide a water hose to wash away liquid hydrocarbons to sewer.
3. Ensure that lines on which valves are to be checked are not in use, and that both ball
valves of the double block are in the fully closed position.
4. Slowly crack open the bleeder valve and allow the section between the valves to
depressure, and any liquid hydrocarbons to drain.
5. If this section cannot be depressured safely, do not attempt to open the bleeder valve
fully. Note this on the Leak Survey Report Sheets.
6. Open bleeder valve and try to estimate the size of any leak (e.g. "none", "very small",
"small", "moderate" and "large"), according to the flow from the Bleeder Knockout
Drum D-2307 on FS-006. Note this, and any other observations, on the Leak Survey
Report Sheets.
7. Once the leak has been estimated, close off the bleeder valve (except the cross-over
bleeder valves, which must be left open when the cross-over is not in use).
8. Repeat Steps 3 through 7 on as many of the lines as possible with the existing drier
line up.
9. Wait until the next time that the line up is reversed and repeat Steps 1 through 8.
3.2 SULFUR STRIPPING

Sulfur poisoning of the I-8 Plus/I-82 catalysts is indicated by loss of isomerization activity
and in a severe case by loss of benzene saturation. If benzene saturation is lost, the lead
reactor temperature differential will shift further down the reactor or be reduced across
the entire reactor. If sulfur poisoning occurs, it is possible to detect H2S in the stabilizer
off gas, although these can be high level HCl interference with H2S detector tubes.
If sulfur poisoning occurs, it is possible to regain activity by stripping the sulfur of the
catalyst. Good recovery has been achieved commercially after the sulfur strip operation.
However, complete recovery should not be expected.
Following is the sulfur stripping procedure:
1. In addition to the normal caustic strength monitoring for % NaOH, the caustic strength
in Net Gas Scrubber T-2302 should be checked frequently to avoid H2S or HCl
breakthrough. The caustic "percent" spent as well as "percent" NaOH (UOP Method
209) should be reported due to the presence of weak acids and bases while
scrubbing H2S and HCl.
2. Discontinue all drier regenerations at a point where the drier being regenerated has
just completed its regeneration cycle.
3. Increase make-up gas flow to the maximum possible.
4. Begin reducing the reactor inlet temperatures to 121°C at a rate of 28°C per hour and
gradually reduce the reactor section pressure to 28 kg/cm2. Leave the charge rate
constant since a sharp reduction could result in high reactor severity and a
temperature excursion.
5. After reducing the temperature and pressure, reduce the feed to the reactors to about
50% of design. Maintain the reactor temperatures at 121°C and maintain maximum
make-up gas flow rate.
6. Discontinue liquid feed to the reactor section. The feed may be routed to the
Stabilizer T-2301 via the start-up bypass 4”-PZ-230130. Feed should be cut out as
quickly as possible to minimize low flow of liquid across the catalyst.
7. Sweep the reactors with maximum make-up gas to remove hydrocarbon from the
catalyst. Hold the reactor temperatures at 121°C and the pressure at 28 kg/cm² g.
Liquid flow from the reactor section will drop off as hydrocarbon is purged. Continue
with these conditions until liquid flow from the reactor section drops off, but for a
minimum of four hours.
8. Increase the make-up hydrogen to the unit to the maximum possible while still
maintaining control of the reactor section and stabilizer pressure.
9. Raise the reactor inlet temperature to 260-315°C. Do not exceed the design limitation
on the heater or any other equipment during this operation. CHECK ALL VENDOR
SPECIFICATION SHEETS. The regeneration electric superheater is used for this
service.
10.Maintain the maximum hydrogen gas flow allowed by the superheater design duty.
11.Continue to inject chloride into the hydrogen purge gas to the reactor, at a rate
equivalent to injecting 100 wt ppm chloride on a design reactor liquid charge basis.
12.Monitor the H2S content of the stabilizer off gas with time. The H2S will slowly
increase to a maximum (perhaps 200-1000 mol ppm, depending on the amount of
sulfur present on the catalyst and the severity of the stripping operation). Over a
period of 12-24 hours, the H2S content will decrease to some fairly stable level.
13.At this point the stripping operation can be considered complete, for practical
purposes.
14.Cool the catalyst bed to 65°C and then stop the purge of drag gas from the product
separator to the stabilizer. Follow the normal start-up procedure to restart feed to the unit.
15.After charging feed to the reactor, adjust the chloride injection rate for 200 wt ppm
based on design liquid reactor charge.
16.Maintain 200 wt ppm chloride injection for 12 hours (minimum); then re-establish the
normal rate of 150 wt ppm based on the liquid reactor charge rate.
17.Figure 3.1 provides an indication of the relationship between reactor inlet temperature
and H2S concentration in the stabilizer off gas over time.
3.3 METHANATOR TEMPERATURE EXCURSION

Temperature excursion
In some cases where high delta T is expected due to the high carbon oxides in the feed,
there is a control system designed to prevent temperature excursions by cutting out the
hydrogen gas feed.
For low levels of carbon oxides there may be only a high temperature alarm which alerts the
operator that attention is needed. In either case, the operator should make sure the feed is
stopped manually and reduce the methanator heater outlet temperature to compensate for
the increase in heat generated. As soon as the temperature is under control, the feed may
be introduced slowly and the reactor inlet temperature controlled accordingly.
If the reactor temperature approaches the vessel limit, take the following actions:
1. Block in the hydrogen gas feed to the reactor.
2. Block in the heating medium to the methanator heater.
3. Block in the methanated gas to the makeup gas driers.
4. Open the warm up vent to the flare and reduce the methanator reactor pressure to 1.5
kg/cm² g less than the nitrogen header.
5. Introduce nitrogen to the reactor at a maximum rate to cool the catalyst bed to a safe
temperature.
Figure 3.1
CHAPTER 8
EMERGENCY SHUTDOWN PROCEDURES
CONTENTS
1. INTRODUCTION
2. EMERGENCY FUNCTIONS PHILOSOPHY

2.1 CONTROL & SAFETY SYSTEMS PHILOSOPHY
2.2 EMERGENCY SHUTDOWN SYSTEMS OF THE PENEX / DIH PROCESS UNIT
3. PROCESS FAILURES
3.1 LOSS OF FEED
3.1.1 PROCEDURE 1
3.1.2 PROCEDURE 2
3.2 LOSS OF MAKE-UP GAS

3.3 HIGH REACTOR TEMPERATURE DIFFERENTIAL
3.3.1 PROCEDURE 1
3.3.2 PROCEDURE 2
3.4 CATALYST PROTECTION PROCEDURES

3.4.1 LIQUID FEED DRIER WATER BREAKTHROUGH
3.4.2 LOSS OF PERCHLOROETHYLENE INJECTION
3.4.3 SULFUR POISONING
3.4.4 HYDROTREATER OPERATION (UNIT 012)
4. UTILITY FAILURES
4.1 INSTRUMENT AIR FAILURE
4.2 COOLING WATER OR FIN-FAN FAILURE
4.3 STEAM FAILURE
4.4 ELECTRICAL POWER FAILURE
5. MAJOR UPSETS
5.1 GENERAL
5.2 UPSETS
5.3 FIRE AND/OR GAS IN THE PLANT
5.3.1 PREVENTION
5.3.2 FIRE AND GAS HAZARD
5.3.3 LEAKING VALVES OR VESSELS

1. INTRODUCTION
Emergencies, which occur in the Penex / DIH Process unit, must be recognized and acted
upon immediately. The operators and supervisory personnel should carefully study in
advance, and become thoroughly familiar with the proper steps to be taken in such
situations. While some of the emergency conditions described here may not result in a unit
shutdown, they could lead to serious damage to equipment if the situation is not handled
properly.
It is strongly recommended that the emergency procedures and the automatic shutdown
systems be understood by all persons involved in the operation. In general, the objective of
the emergency procedures is to avoid damage to equipment.
Specific rules cannot be made to cover all situations, which might arise. Therefore, the
following procedures cover only those emergency situations, which are the most common,
and, for the most part, only the immediate steps to be taken are listed.
It should also be noted that the protection of austenitic stainless steel equipment must
always be kept in mind. The proper precautionary measures must be taken to prevent
oxygen and liquid water from coming into contact with any austenitic material that has
sulfidic scale. These measures should not conflict with the immediate steps required as a
result of the emergency condition.
2. PROCESS FAILURES
2.1 LOSS OF FEED

Loss of feed to the PENEX Reactor (R-2302/2303) is an emergency situation. When feed
flow stops, the feed, which is in the reactor circuit, will flow through the reactor at a low
LHSV. The feed will be swept through the reactor by the make-up gas. The feed could be
heated to a high temperature, by the Charge Heater (E-2308), if the charge rate drops
suddenly. The reactor pressure will drop as a result of the throughput reduction which will
cause the back pressure control valve to close off (PIC-097). The combined effect of these
responses to a loss of feed is high reactor severity, which could result in overconversion of
the feed and a reactor temperature excursion. The procedure below will minimize the
possibility of a temperature excursion occurring when feed is lost.
Two loss of feed procedures are detailed below. Procedure 1 is for complete loss of feed,
such as if the Charge Pumps (P-2301 A/B) cannot work. Procedure 2 is for low feed
availability, such as loss of feed from the hydrotreater.
2.2 PROCEDURE 1
When feed flow is lost:
1. Stop the flow of steam to the Charge Heater (E-2308). This should happen automatically
when the feed flow drops below the charge heater shutdown point.
2. Increase the make-up gas flow to maximum. Route the make-up gas to the lead reactor
inlet purge line, via HV-012.
3. Slowly depressure the reactor circuit to the Stabilizer (T-2301). Depressure at a rate,
which allows stable pressure control of the stabilizer.
4. Stop C2CI4 injection when the lead reactor temperature is 105°C.
5. Observe the reactor temperatures. If the temperatures are below 232°C and stable,
continue with the make-up gas purge and cooldown the reactor to 65°C. If depressuring
to 3.5 kg/cm² above the stabilizer does not stop the temperature excursion, depressure
the reactors to the flare. Cooldown the unit and restart according to the normal start-up
procedure.
2.3 PROCEDURE 2
If feed is lost to the PENEX unit battery limits or if for some reason low feed flow (lower
than required to maintain 0.5 LHSV overall) is expected, then open the emergency
circulation line 3”-PL-230255 to the liquid Feed Driers (DR-2303/2304), flow controlled by
FIC-032. This action will prevent an emergency shutdown of the reactor circuit.
2.4 LOSS OF MAKE-UP GAS

When make-up gas flow is lost, there will be a drop in reactor pressure and an increase in
reactor liquid content. This will result in an increase in reactor residence time, which could
result in more complete isomerization of feed and possibly cause a reactor temperature
excursion. The loss of make-up gas also increases the risk of catalyst coking. If make-up
gas flow is lost for a short time, the unit can be secured by reintroducing the gas.
If the loss of make-up gas is long term, the unit will have to be shutdown since it will
eventually not be possible to isomerize the feed without hydrogen present. Also it may not
be possible to maintain circulation. Circulation cannot be maintained because there will be
no pressuring medium for the stabilizer to move stabilizer bottoms. If there is a long-term
loss of make-up gas, proceed as follows:
1. Methanator heater (A-2302) will be automatically shutdown and steam flow to the
Charge Heater (05 E 10) will be stopped automatically by Methanator Heater Shutdown
023-UX-013.
2. Stop the C2CI4 injection when the lead reactor temperature reaches 105°C.
3. Slowly depressure the reactor circuit to 24.6 kg/cm² g to keep the back pressure
Control Valve (PV-097) open and feed flowing through the reactors.
4. Maintain feed flow as long as a level can be controlled in the bottom of the Stabilizer (T-
2301). If the make-up gas is still available at a low pressure, and if the pressure is high
enough to keep pressure on the stabilizer, open the pressuring line to the stabilizer. The
stabilizer pressure can be reduced to achieve pressure control on the column and flow
of bottoms.
5. Cool the reactor to 93°C and remove feed. If circulation cannot be maintained, cool the
reactor circuit as much as possible and remove the feed.
6. Restart the unit following the normal start-up procedure.
7. If the reactor temperatures climb above 232°C during this procedure, stop the feed,
block in the reactor and depressure the reactor to the flare.
2.5 HIGH REACTOR TEMPERATURE DIFFERENTIAL

A high reactor temperature differential could result from the presence of larger than normal
amounts of benzene, olefins or C7+ material in the feed. Or a high reactor temperature
differential could result from high catalyst severity, i.e. low throughput and too high of a
temperature for the feedrate being maintained.
In order to avoid a reactor temperature excursion:
1. Avoid low reactor liquid feedrates. The reactors should never be operated below 0.5
LHSV overall (1 LHSV per reactor).
2. Avoid large quantities of benzene, olefins or C7+ in the feed. Limits on these materials in
the feed depend on the unit design. Typical limits are:
a. Benzene - 5%
b. Olefins - 2%
c. C7+ - 5%
3. Avoid overheating the reactor charge.
During an emergency such as a power failure or instrument air failure, it will be difficult if
not impossible to avoid 1. and 3. above. The emergency procedures are written with the
possibility of a reactor temperature excursion in mind.
Following are the procedures for high reactor temperature differential. There are two different
procedures depending on the cause of the temperature excursion. If the temperature
excursion was caused by an increase in feedstock benzene, olefins or C7+, Procedure 1 is
used. If the excursion is the result of cracking (usually due to low throughput) then
Procedure 2 is used.
2.6 PROCEDURE 1
If the lead reactor temperatures increase and the increase did not coincide with low reactor
throughput, loss of make-up gas or an excessively high reactor inlet temperature, then the
high temperatures are probably the result of an increase in the reactor feed benzene,
olefins or C7+ content. The procedure is as follows:
1. Stop flow of steam to the Charge Heater (E-2308). Reduce the reactor inlet
temperatures to 105°C.
2. Open the lead reactor purge valve and establish design flow to the lead reactor inlet and
increase the make-up gas flow to maximum. This will accelerate the rate of reactor
cooldown.
3. Stop chloride injection when the lead reactor temperature drops to 105°C.
4. Modify upstream fractionation conditions to remove the benzene and other heavy
materials from the PENEX feed. Consider use of the emergency recirculation line 3”-PL-
230255 (de-isohexanizer to liquid feed driers).
5. Stabilize the unit and increase the reactor inlet temperatures as the temperature
differential in the lead reactor comes down.
6. If any of the reactor temperatures increase above 232°C, proceed to Procedure 2, step
5.
2.7 PROCEDURE 2
If the reactor temperature differential increases and the increase coincides with a reduction
in charge rate or an increase in reactor inlet temperature, the reactor severity is too high
causing the temperature excursion. When any of the reactor bed temperatures get over
204°C, immediate action must be taken. The procedure is as follows:
1. Stop flow of steam to the charge heater (E-2308) to remove heat input.
2. Open the reactor purge valve to the lead reactor inlet and increase the make-up gas flow
to maximum. This will accelerate the rate of reactor cooldown and reduce the reactor
residence time.
3. Ensure that the feedrate to the reactor is equivalent to at least 0.5 LHSV across the unit
or 1 LHSV per reactor. Use the emergency recirculation line 3”-PL-230255 (de-
isohexanizer to the driers) to increase charge if fresh feed is not available.
4. Stop the chloride iniection.
5. Slowly depressure the reactor circuit to the Stabilizer (T-2301). Depressure the
stabilizer to 3.5 kg/cm² above the Caustic Scrubber (T-2302) to allow the reactor circuit
to be depressured to the lowest possible pressure without venting to the flare.
6. When the reactors have been depressured, monitor the reactor temperatures. If the
reactor temperatures are increasing and are above 232°C, do the following:
§ Remove the liquid feed.
§ Block in the lead reactor inlet and the make-up gas purge line.
§ Block in the stabilizer feed line at the reactor pressure control valve PV-097.
§ Depressure the reactors to the flare from the outlet of the lag reactor. Depressure to
a pressure of 3.5 kg/cm² g.
§ The reactors can be cooled by purging with dry oxygen-free nitrogen. The nitrogen
can be routed through the gas driers, if required, to ensure dryness.
§ Restart the unit following the normal start-up procedure once the reactors have been
cooled below 65°C.
7. If, after step 5, the reactor temperatures are decreasing below 232°C then:
§ Restart the chloride injection.
§ Cooldown the reactors to the normal operating temperature.
§ Raise the reactor pressure to a normal level.

§ Decrease the make-up gas flow to a normal level.
§ Establish normal operations.
2.8 CATALYST PROTECTION PROCEDURES

Following are some guidelines regarding protection of the PENEX catalyst. These
guidelines are being provided in addition to the information covered in the normal operating
and emergency procedure sections of this manual.
2.8.1 LIQUID FEED DRIER WATER BREAKTHROUGH

If water breaks through a Feed Drier (DR-2303/2304), as indicated by the Moisture
Analyzer (AT-001 B) located at the lead drier outlet, immediate action must be taken.
Generally the driers are taken off-line and regenerated on a timed schedule rather than on
water breakthrough. Water breakthrough is considered an unusual occurrence.
Water entry to the reactor circuit will cause irreversible catalyst damage. The moisture
analyzer is the only warning available of water entry to the unit and it must be assumed to
be reading correct if breakthrough occurs. Any debate regarding its accuracy should be
made only after the feed or make-up gas has been removed from the reactor circuit.
If the feed or gas are cut out, the appropriate loss of feed or loss of make-up gas
emergency procedure must be followed.
After the unit has been secured, the drier, which experienced the breakthrough, should be
regenerated. The moisture analyzer should be checked and the regenerated drier effluent
analyzed to verify the water removal capability. If the drier is not capable of removing water
after a proper regeneration procedure, the drier temperature and water content should be
checked. The driers will not function properly if the feed contains a large quantity of free
water. If no other problems can be found, the drier must be opened and inspected for
problems such as channeling. If no disturbance of the bed is noticed, it is possible that the
drier sieve was contaminated. If the drier sieve does not function properly it must be
reloaded with fresh sieve.
2.8.2 LOSS OF PERCHLOROETHYLENE INJECTION

If C2CI4 injection is lost, chloride will be stripped from the catalyst resulting in a loss of
catalyst isomerization activity. The stripping action will increase at higher temperature and
throughput. If chloride is lost for only a few hours (less than 6 hours), the catalyst activity
can be regained by resuming chloride injection. If the chloride stripping is continued for a
long period of time (more than 6 hours), the ability for the catalyst to regain activity is
reduced and irreversible catalyst damage results.
If, after losing chloride, it appears that chloride will not be available for more than 6 hours
the unit should be shutdown. After 4 hours of operation preparations for shutdown should
be made. If chloride is lost the reactor temperatures then feedrate should be reduced to
minimize stripping. Operation at 50% of design feedrate is recommended.
When chloride is made available, the chloride injection rate should be maintained at 300 wt
ppm until the stabilizer off gas chloride content increases back to its normal level.
2.8.3 SULFUR POISONING

Sulfur poisoning of the I-8 Plus/I-82 catalysts is indicated by loss of isomerization activity
and in a severe case by loss of benzene saturation. If benzene saturation is lost, the lead
reactor temperature differential will shift further down the reactor or be reduced across the
entire reactor. If sulfur poisoning occurs, it is possible to detect H2S in the stabilizer off
gas, although high HCl tends to interfere with H2S detector tubes. If in the caustic, the
Na2S concentration increases this indicates high sulfur levels.
If sulfur poisoning occurs, it is possible to regain activity by stripping the sulfur of the
catalyst. Good recovery has been achieved commercially after the sulfur strip operation.
However, complete recovery should not be expected.
1. Discontinue all drier regenerations at a point where the drier being regenerated has just
completed its regeneration cycle.
2. Increase makeup gas flow to the maximum possible.
3. Reduce the reactor inlet temperatures to 121°C at a rate of 28°C per hour. Leave the
charge rate constant since a sharp reduction could result in high reactor severity and a
temperature excursion.
4. When the reactor temperatures reach 121°C, decrease the charge rate slowly to 50
percent of design flow in increments of 5% of scale every 15 minutes. Maintain the
reactor temperatures at 121°C and maintain at least the design flow of makeup gas
through the reactors.
5. After the charge rate has been reduced, depressure the reactor circuit to 21 kg/cm² g.
Depressure at a rate which allows stabilizer pressure to remain in control.
6. After depressuring to 21 kg/cm² g, discontinue feed to the unit. The feed may be routed
to the stabilizer (T-2301) via start-up bypass 4”-PZ-230130. Feed should be cut out as
quickly as possible to minimize low flow of liquid across the catalyst.
7. Maintain at least the design lfow of makeup gas to the reactors. Hold the reactor
temperatures at 121°C and the pressure at 21 kg/cm² g. Sweep the reactors for at least
four hours at these conditions to remove hydrocarbon from the catalyst.
Note: Lower pressures may be used for sulphur stripping but it is generally not
recommended to reduce the reactor pressure below the charge heater heating medium
(steam or hot oil usually) pressure to avoid potential leakage from the charge heater into the
reactors. If the regenerant superheater is used for sulphur stripping, the charge heater heat
source should be blocked in and depressured. If the charge heater is required for sulphur
stripping, it is recommended to leak test the charge heater tube bundle prior to performing
the sulphur strip.
8. Raise the reactor inlet temperature to 260-315°C. Do not exceed the design limitation
on the heater or any other equipment during this operation. CHECK ALL VENDOR
SPECIFICATION SHEETS. The regeneration electric superheater is typically used for
this service.
9. Maintain maximum hydrogen gas flow allowed by the superheater design duty.
Minimize the amount of heavier hydrocarbon in the makeup gas if possible to reduce
the chance of a temperature excursion during stripping.
10. Continue to inject chloride into the hydrogen purge gas to the reactor, at a rate
equivalent to injecting 100 wt ppm chloride on a design reactor liquid charge basis.
11. Consistent with maintaining normal operating pressure, increase the makeup gas
hydrogen to maximum, venting off the stabilizer through the scrubber.
12. Monitor the H2S content of the stabilizer offgas with time. The H2S will slowly increase
to a maximum (perhaps 200-1000 mol ppm, depending on the amount of sulphur
present on the catalyst and the severity of the stripping operation). Over a period of 12-
24 hours, the H2S content will decrease to some fairly stable level.
13. At this point the stripping operation can be considered complete, for practical purposes.
14. Cool the catalyst bed to 65°C and begin charging feed to the unit again according to the
normal start-up procedures.
15. After charging feed to the reactor, adjust the chloride injection rate for 200 wt ppm on
feed.
16. Maintain 200 wt ppm chloride injection for 12 hours (minimum); then re-establish the
normal rate of 150 wt ppm based on the reactor charge rate.
2.8.4 HYDROTREATER OPERATION (UNIT 012)

If the hydrotreater reactor (Unit 012) shuts down or if there is an upset in the hydrotreater
which causes the reactor temperatures to drop below the level required to properly treat the
feed, there is a risk that catalyst poisons will not be removed and the feed must be
removed from the P E N E X unit.
The PENEX unit should be shutdown in as orderly a manner as possible, however, the
longer the contaminated feed passes over the catalyst, the more likely permanent catalyst
damage will occur. If the only contaminant is sulfur there is the possibility of recovery.
Oxygenates, metals and nitrogen will permanently deactivate the catalyst.
3. UTILITY FAILURES
3.1 INSTRUMENT AIR FAILURE

In case of loss of instrument air, the operation of the Penex / DIH Process Unit will become
out of control as the pneumatic operated valves go to their safety position (fail close or fail
open). This is not necessarily the same position as when the plant is being shutdown
according to normal shutdown procedures.
If there is a plant-wide air failure, the chances are that the unit will have to be shutdown.
This will be the safest way to proceed. If the reason for the failure can be located quickly, a
shutdown may be prevented. For example if the shutdown is the result of failure of the air
drying section, that section can be bypassed and repaired.
If the air fails to one or two valves, operation could perhaps proceed using a bypass. This
ability depends on the service. Operating with a manual bypass will require constant
operator attention.
If there is an instrument air failure and the air pressure cannot be regained, proceed as
follows:
♦ Ensure that all heat inputs are shut-off to prevent overheating and overpressuring. The
Methanator Heater (A-2302), the Reactor Charge Heater (E-2308), the stabilizer and De-
isohexanizer Reboilers (E-2309 and E-2316) should be shutdown and the steam supply
blocked in. Also Regenerant Vaporizer (E-2305) and Regenerant Superheater (A-2301) if
it is in service.
♦ Stop chloride injection.
♦ In general spillback and reflux valves will fail open. The reactor effluent pressure control
valve PV-097 will fail in position. Most other valves will fail closed. For the valves which
fail closed, make sure the associated block valves are closed. This will prevent loss of
control if air pressure is regained.
♦ The reactor circuit should be depressured to the Stabilizer (T-2301) to remove
hydrocarbon from the reactors and minimize the potential for high reactor severity.
Since the reactor back pressure control valve PV-097 fails in position, the reactor circuit
will depressure to the stabilizer as soon as air fails and feed and make-up gas are lost.
Block in the lead reactor inlet using the Emergency Block Valve (XV-092) to prevent
feed from entering the reactors from the feed circuit when the reactors are depressuring.
♦ The stabilizer and scrubber pressures will have to be manually controlled, using the
control valves PV-022 and PV-024 bypasses since these valves fail closed.
♦ If, during the instrument air failure, the reactor temperatures climb above 232°C, block in
the reactors and depressure to the flare. Depressure to 3.5 kg/cm² g.
♦ When air pressure is regained and if the reactor temperatures are below 232°C,
establish maximum make-up gas flow to the lead reactor inlet via the Hydrogen Purge
Line (HV-012).
3.2 COOLING WATER OR FIN-FAN FAILURE

Coolers are located on the methanator outlet to the makeup gas driers (E-2303), Stabilizer
Overhead (E-2310 and E-2311), De-isohexanizer Overhead (E-2317 and E-2318), the DIH
sidedraw (E-2313 and E-2314) and the product streams (E-2315). If the coolers stop
working, there will be overpressuring in the Stabilizer (T-2301) and De-isohexanizer (T-
2303). If the driers operate too hot, the water retention capability is reduced, jeopardizing
the I-8 Plus/I-82 catalysts. If products cannot be cooled properly there is a risk of
overheating storage tanks and causing a fire hazard. Do not send hot naphtha (> 50°C) to
storage.
If cooling water fails for an extended period of time, the unit will need to be shutdown using
an accelerated shutdown procedure. The procedure follows. This procedure assumes that
the stabilizer condenser has been lost and cannot be restarted.
1. Stop the flow of steam to the Charge Heater (E-2308).
2. Maintain make-up gas flow and reactor feed.
3. Stop chloride injection when the lead reactor temperature is 105°C.
4. Reduce the heat input to the stabilizer and De-isohexanizer Reboilers (E-2309 and E-
2316) to maintain the stabilizer and de-isohexanizer pressures.
5. Follow the normal shutdown procedure as closely as possible.
3.3 STEAM FAILURE

If steam is lost, the PENEX unit and De-isohexanizer (T-2303) must be shutdown. Steam is
used in the Reactor Charge Heater (E-2308), the stabilizer and De-isohexanizer Reboilers
(E-2309 and E-2316). Since the stabilizer reboiler will stop functioning, unstabilized product
could be produced if feed is continued to the unit. To stop the production of unstabilized
product, the feed must be removed from the unit. The procedure is as follows:
NOTE: The Stabilizer (T-2301) and DIH column (T-2303) pressures will fall quickly due to
the loss of heat. Stop fin-fan coolers as required and shutdown reflux pumps as levels fall
below 50%. However, do not allow the overhead drums to overfill.
1. Increase the make-up gas flow to maximum. Open the lead reactor inlet make-up gas
purge line (HV-012) to accelerate cooldown. Establish design flow on the hydrogen
purge line.
2. Stop chloride injection.
3. Remove feed from the reactor circuit and immediately depressure the reactors to the
stabilizer. Drop the pressure to 3.5 kg/cm² above the stabilizer.
4. Cool the reactors down to 65°C.
5. When steam is regained, restart the unit.
6. If during the heating failure procedure the reactor temperatures climb above 232°C, the
reactors must be depressured to as low a pressure as possible. If the reactors have
been depressured as far as possible to the stabilizer and the reactor temperatures are
over 232°C and climbing, then the reactors must be depressured to the flare.
3.4 ELECTRICAL POWER FAILURE

If electrical equipment fails, all electrically driven equipment, pumps, compressors, fin-fans,
etc. will stop. Due to the loss of flow through the reactors, which results from the power
failure, a severe condition will exist in the reactor, which could result in a temperature
excursion. The immediate concern is to remove hydrocarbon from the reactor and to lower
the pressure.
The procedure is as follows:
1. Block in the steam to the Reactor Charge Heater (E-2308), the Stabilizer Reboiler (E-
2309), De-isohexanizer Reboilers (E-2316) and Regenerant Vaporizer (if in service) (E-
2305).
2. Restart cooling water pumps and fin-fans, if possible.
3. Block in the lead reactor inlet using the Board Mounted Switch (XV-092).
4. Depressure the reactors to the stabilizer to remove hydrocarbon from the reactors.
Depressure the stabilizer to 3.5 kg/cm² above the caustic scrubber (T-2302). The
reactor circuit should be depressured at a rate which avoids lifting of the stabilizer
safety valve.
a. If instrument air has also failed, the Reactor Back Pressure Control Valve (PV-097)
should fail in position. This position may or may not be adequate for
depressurization of the reactor circuit at the desired rate. The Back Pressure Control
Valve (PV-097) is equipped with a bypass so that the rate of depressurization can be
changed if necessary. Air failure will require that the stabilizer and scrubber be
depressured manually using the Control Valve Assembly Bypasses using first PIC-
024 followed by PIC-022.
b. If the reactor cannot be depressured to the stabilizer, then depressure to the flare
system. Whenever the reactors are depressured to the flare, the Lead Reactor Inlet
(XV-092), hydrogen purge lines (1½”-PG-230154 and HV-012) and Back Pressure
Control Valve Station (PV-097) should be closed.
5. If possible establish a hydrogen purge across the reactors to accelerate cooldown. The
hydrogen purge line, which is routed to the lead reactor inlet, should be used. HV-012
has a hand jack, which can be used to open the valve.
6. Continue depressuring to the stabilizer until the reactors have been depressured as low
as possible. Maintain the purge if available and cool the reactors to 65°C.
7. If, after depressuring to the stabilizer, the reactor temperatures climb above 232°C, then
depressure to the flare. When depressuring to the flare, do so from the lag reactor outlet
via XV-093 A and B. Block in the Reactor Back Pressure Control Valve (PV-097), and
the hydrogen purge lines (1½”-PG-230154 and HV-012).
8. After cooling the reactors to 65°C, restart the unit following the normal start-up
procedure.
4. MAJOR UPSETS
4.1 GENERAL
In a modern plant several different substances are present, that can, when handled
improperly, become hazard for the personnel and the installation.
It is necessary that each operator is familiar with the nature of the material in his area(s),
that he knows the hazard to his own and to other people's health, the fire risk or explosion
danger, and that he knows which protective measures to take.
The best protection against all hazards is prevention. It is an essential part of the task of
each operator to prevent the forming of a hazardous situation.
However, there are always situations that a hazardous situation has developed.
When a hazardous situation has developed the operator must apply all means available to
prevent accidents to personnel and to damages to equipment
This hazardous situation is causing a major upset in a production process.
4.2 UPSETS
Major upsets can be a result of:
♦ Serious leaks in the installation (pump seal, flanges, connections, etc.)
♦ Line ruptures, tube ruptures in heater.
♦ Chemical reaction
♦ Fire
♦ Explosions
In case one of this major upsets occurs, the first action will be to prevent accident to
personnel, followed by prevent to damage of equipment.
If possible isolate the problem area, depressurize when possible and necessary.
In case of a major hazardous situation:
♦ Sound alarm and notify proper services.
♦ Stop hydrocarbon and gas feed to the unit and stop all heat input.
♦ Depressure the plant to the flare and try to isolate the effected area.
♦ Shutdown the remainder of the equipment as the situation permits.
Some special considerations regarding the PENEX unit in an emergency:
♦ The unit contains light hydrocarbons and hydrogen, which are explosive and/or highly
flammable.
♦ The unit contains benzene and perchloroethylene, which are known health hazards.
♦ The unit contains HCl downstream of the reactor 1 inlet. The concentration is
particularly high in the stabilizer overhead.
♦ Benzene and olefins in the PENEX feedstock will saturate in the reactor. Much of the
C7+ will hydrocrack. The saturation and cracking reactions are exothermic. If the levels
of these components in the feed increase significantly, the heat produced could raise
the lead reactor temperature beyond the normal operating range.
♦ A reactor temperature excursion could occur if the flow of liquid through a hot reactor is
too low or if the reactor temperatures are too high. Each reactor LHSV should always
be kept above 1.0 Hr. -I.
♦ The Caustic Scrubber (T-2302) vents to a system, which runs under pressure. During an
emergency the Stabilizer (T-2301) could depressure below the scrubber pressure. There
is a check valve in the stabilizer off gas line. However, if the check does not hold, water
and caustic could back up into the stabilizer causing a potential corrosion problem.
There is a double block and bleed on the line which should be closed once gas flow
from the stabilizer stops.
♦ If a reactor temperature excursion occurs and temperatures climb above 232°C, the
reactors must be depressured to prevent mechanical damage. At the usual outlet
operating pressure of 31.6 kg/cm² g, the reactor design temperature is typically 260°C.
Action should be taken before the temperature climbs to the point that mechanical
problems could occur.
♦ During a temperature excursion, the reactors should be depressured. If for some reason
the reactors cannot be depressured to the stabilizer or if after depressuring to the
stabilizer the reactor temperatures are over 232°C and climbing, then the reactors
should be depressured to the flare. Whenever the reactors are depressured to the
flare, the Lead Reactor Inlet (XV-092), the hydrogen purge quench lines (1½’-
PG-230154 and HV-012) and the Reactor Back Pressure Control Valve Station
(PV-097) should be blocked in.
Exact procedures cannot be provided for every type of emergency situation. General
procedures for the most common types of emergency situations follow. With an
understanding of these procedures and the various concerns outlined above, the operators
should be able to devise a course of action for the various situations that can arise.
4.3 FIRE AND/OR GAS IN THE PLANT
4.3.1 PREVENTION
Due to the fact that among the product there are combustion and hazardous materials, it is
necessary to:
a. Eliminate from the plant all possible physical hazards that may result in injuries to
worker or damage to equipment.
b. Reduce fire hazard to a minimum.
c. Introduce accident prevention measures.
d. Make safety a prime function of each employee.
The chief factors in carrying on safety work are:
a. Availability of adequate rules and regulations.
b. Familiarity of all personnel with the rules and regulations. Adequate and continuous
education in safety.
c. Rigid enforcement of these rules and regulation.
d. Availability and use of safety clothing and other protective equipment for hazardous
activities.
e. First aid equipment and personnel trained in first aid.
f. An adequately equipped fire-fighting system.
4.3.2 FIRE AND GAS HAZARD

When combustible gases are mixed with oxygen (air), an explosive mixture may be
formed. Whether such a mixture is explosive depends on the concentration of the gas in
the gas-air mixture.
The concentration below and above which the mixture is not explosive are called the lower
and higher explosion limits, respectively. In the book for "dangerous properties of industrial
materials" published by Van Nostrand RENOLDS Company N.Y.
Since there are no plant interlocks with the fire and gas detection system in the plant,
action to be taken on detection of fire and/or gas in the plant are purely manual and to be
executed in accordance with all safety rules and with the company's fire and gas safety
regulations and philosophy and with the chief factor to avoid injuries to personnel.
If possible the source of the fire and/or gas escape shall be isolated or a total plant shut
down can also be initiated by detection of fire at the respective vessel.
If possible all inventories in the fire area shall be reduced till minimum.
4.3.3 LEAKING VALVES OR VESSELS

Leaking valves and vessels in the sections of the plant which contain HCl are considered
an emergency since the contact of HCl with the atmospheric moisture can cause rapid
corrosion. Leaks should be repaired quickly.
CHAPTER 9
SAFETY EQUIPMENT AND PROCEDURES
CONTENTS
1 PRESSURE SAFETY DEVICES
2 ALARM SETTINGS
3 TRIP SETTINGS
4 TRIP SYSTEM CHART
5 CAUSE AND EFFECT DIAGRAM
6 MATERIAL HAZARD DATA SHEETS
7 SAFEGUARDING MEMORANDUM
1 PRESSURE SAFETY DEVICES

Refer to the following documents:
8474L-200-NM-0006-001 Flare Discharge Summary – NHT / CCR / ISOM

In Tools specifications of safety valves
2 ALARM SETTINGS
Extract from I/O list of all instruments with alarm and alarm values will be attached in this
paragraph
3 TRIP SETTINGS
Extract from I/O list of all instruments with trip function will be attached in this paragraph
4 TRIP SYSTEM CHART
Refer to Cause and Effect Chart attached in Chapter 9.5 and Trip Setting list attached in
Chapter 9.3.
5 CAUSE AND EFFECT DIAGRAM

Refer to the following document:
8474L-023-DW-1514-201 Cause and Effect Chart – Unit 023

6 MATERIAL HAZARD DATA SHEETS
MSDS of Chemicals and catalyst will be attached in this paragraph.

7 SAFEGUARDING MEMORANDUM
HAZOP Action 2262: Sour Gas Sampling procedure is described chapter 12.
CHAPTER 10
INSTRUMENT DATA
CONTENTS
1 CONTROL VALVES AND INSTRUMENTS
2 ORIFICE PLATES
1 CONTROL VALVES AND INSTRUMENTS

8474L-023-SP-1541-001 Control Valves
8474L-023-SP-1543-001 Pneumatic Ball Valves
8474L-023-SP-1543-006 On-Off Ball Valves
8474L-023-SP-1547-002 Rotameters
8474L-023-SP-1547-008 Thermal Mass Flowmeters
8474L-012-SP-1553-002 Electronic DP Flowmeters
Control valves datasheets issued by In Tools
Flow instrument datasheets issued by In Tools
2 ORIFICE PLATES
Orifice plate datasheets issued by In Tools
Restriction orifice datasheets issued by In Tools
CHAPTER 11
SUMMARY OF MAJOR EQUIPMENT
CONTENTS
1 EQUIPMENT LIST
2 LARGE ROTATING EQUIPMENT
3 HEATERS
4 OTHER VENDOR INFORMATION

1 EQUIPMENT LIST
8474L-200-EL-001 POC Project Equipment List
2 LARGE ROTATING EQUIPMENT

N/A
3 HEATERS
N/A
4 OTHER VENDOR INFORMATION
Vendor list of instruments with alarm and trip set points of compressors, heaters and important packages
CHAPTER 12
ANALYSIS
CONTENTS
1. INTRODUCTION
3.1 GENERAL
3.2 SAMPLES FOR UOP ANALYSIS
3.3 SAMPLE CONTAMINATION - CONTAINER PROBLEMS
3.4 MINIMUM SAMPLE SIZE IF SENT TO UOP FOR ANALYSIS
4. ON LINE ANALYSERS
1. INTRODUCTION
The attached tables are a guideline for planning sound analytical control of plant
operation during start-up and normal operation.
In the tables are listed:
♦ streams to be analyzed;
♦ analyzes to be performed;
♦ frequency of analysis during start-up and normal operation.
In this section, all recommended test methods are those which are the most applicable
for control analysis by plant personnel. The methods have been selected for their
simplicity, rapidity and convenience with minimum sacrifice of accuracy.
The analytical results will often determine whether the material has to be "off-graded", or
whether the material is acceptable for the next processing step. Therefore, it is obvious
that ever precaution should be taken to make the sample representative of the original
material. That is, it must be like all the rest of the material being processed or the material
collected in the vessel.
The analytical results reported by the laboratory can be no better than the sample
submitted. An analysis or test however, efficiently carried out, will be rendered valueless
if the sample has been improperly taken.
Absolute verification of out-of-specification batches of material must be made by re-
sampling and repeating the analysis before the material is off-graded.

Refer to the enclosed table “Laboratory Schedule for Process and Utility Units – Unit 023
– Isomerization” hereafter called Table 1.
Certain feedstock and product analyses are required in order to monitor plant
performance. The streams that must be analyzed and typical analyses for those streams
are shown in the tables attached. The list does include all tests that are needed to
assure the feed is suitable charge stock to the unit and all the tests that are needed to
complete a hydrogen weight balance around the plant.
Table 1 indicates a sampling frequency for each test. This is very subjective and is
intended to give the refiner a rough idea of how much laboratory work will be needed.
With experience, the frequency of the tests may be optimized. Some of the tests may
also be omitted if they are not relevant to the refiners operation.
The tests marked "D" (Daily) are tests which should be run frequently primarily to keep
the products on specification. The tests marked "W' (Weekly) are tests which only need
to be run occasionally. These tests will be for monitoring plant performance beyond the
day to day operation and for checking that the feed quality is adequate for maintaining
catalyst stability. The tests marked "On request" are tests that are needed only during
test runs to obtain a hydrogen weight balance on the unit.
The analyses shown include all tests that are part of the guarantee agreements.
The PID for details of sample connections (8474L-023-PID-0021-060) is enclosed in §2
of Chapter 14.
TABLE 1 - LABORATORY ANALYTICAL SCHEDULE FOR PROCESS AND UTILITY UNITS UNIT 023 - ISOMERIZATION
Frequency
Item TAG / Type PID Stream / Location Analysis Test Method
Normal Start Up
SCC-2301 012-PID-0021-036 Fresh Feed / 012-FV-026 Composition, wt-% UOP 551 1/D 3/D
(Use SCC-1207 / 21 Total Sulfur, wt-ppm UOP 727 or 1/D 3/D
in NHT Unit 012) ASTM D 4045
Total Nitrogen, wt-ppm UOP 384 or 1/W 3/D
ASTM D 4629
Total Chlorides, wt-ppm UOP 395 Occas. 1/D
Water, wt-ppm UOP 481 1/W 1/D
Dissolved Oxygen, wt-ppm UOP 678 Occas. Occas.
Oxygenates UOP 960 Occas. 1/D
Arsenic, wt-ppb UOP 296 Occas. Occas.
UOP 387 (alt)
Lead, wt-ppb UOP 350 Occas. Occas.
Mercury, wt-ppb UOP 938-95 Occas. Occas.
Copper, wt-ppb UOP 144 Occas. Occas.
Fluoride, wt-ppm UOP 619 Occas. Occas.
RON-clear ASTM D 2699 1/W 1/D
MON-clear ASTM D 2700 Occas. Occas.
Bromine Number UOP 304 or Occas. Occas.
ASTM D 1492
SC-2302 / 1B 023-PID-0021-017 Reactor Charge / 023-FV-009 Composition, wt-% UOP 551 Occas. Occas.
Total Sulfur, wt-ppm UOP 727 or Occas. Occas.
ASTM D 4045
Total Nitrogen, wt-ppm UOP 384 or Occas. Occas.
ASTM D 4629
Total Chlorides, wt-ppm UOP 395 Occas. Occas.
Water, wt-ppm UOP 481 Occas. Occas.
Dissolved Oxygen, wt-ppm UOP 678 Occas. Occas.
Oxygenates UOP 960 Occas. Occas.
Arsenic, wt-ppb UOP 296 Occas. Occas.
UOP 387 (alt)
Lead, wt-ppb UOP 350 Occas. Occas.
Mercury, wt-ppb UOP 938-95 Occas. Occas.
Copper, wt-ppb UOP 144 Occas. Occas.
Fluoride, wt-ppm UOP 619 Occas. Occas.
RON-clear ASTM D 2699 Occas. Occas.
Bromine Number UOP 304 or Occas. Occas.
ASTM D 1492
SC-2303 / 3B 023-PID-0021-019 Lead Reactor Effluent / Outlet R-2302/2303 Composition, wt-% UOP 551 1/W 1/D
SCC-2304 / 21 023-PID-0021-026 Stabilizer Bottoms (DIH Feed) / 023-LV-007 Composition, wt-% UOP 551 1/D 1/D
RON-clear ASTM D 2699 1/D 1/D
MON-clear ASTM D 2700 As Req. As Req.
RVP ASTM D 323 1/D 1/D
HCl UOP 395 1/D 3/D
SC-2305 / 4 023-PID-0021-010 Makeup Gas to Methanator / Inlet E-2301 Composition, mol-% UOP 539 1/W 1/D
(Sample in Total Sulfur, mol-ppm UOP 212 or 1/D 1/D
Platformer) Draeger Tube
Basic Nitrogen, mol-ppm UOP 430 Occas. 1/D
Water, mol-ppm ** Cont. Cont.
CO/CO2, mol-ppm UOP 603 1/W 1/D
HCl, mol-ppm UOP 232 or 1/W 1/D
Draeger Tube
SC-2306 / 4 023-PID-0021-010 Makeup Gas from Methanator / Outlet E-2303 Composition, mol-% UOP 539 Occas. Occas.
Total Sulfur, mol-ppm UOP 212 or Occas. Occas.
Draeger Tube
Basic Nitrogen, mol-ppm UOP 430 Occas. Occas.
HCl, mol-ppm UOP 232 or 1/W 1/D
Draeger Tube
SC-2307 / 4 023-PID-0021-011 Makeup Gas from Methanator / Outlet DR-2301/2302 Composition, mol-% UOP 539 Occas. Occas.
Total Sulfur, mol-ppm UOP 212 or Occas. Occas.
Draeger Tube
SC-2308 / 2 023-PID-0021-021 Stabilizer Off-Gas / 023-PV-022 Composition, wt-% UOP 539 1/D 1/D
H2S, mol-ppm UOP 212 or Occas. Occas.
Draeger Tube
HCl, mol-ppm Draeger Tube Occas. Occas.
SC-2309 / 2 023-PID-0021-022 Net Gas Scrubber Off-Gas / 023-PV-024 Composition, mol-% UOP-539 1/W 1/D
HCl, mol-ppm Draeger Tube 1/D 3/D
SC-2310 / 1B 023-PID-0021-023 Circulating Caustic / P-2307 A/B NaOH, wt-% UOP 209 1/D 1/D
SC-2311 / 15 023-PID-0021-023 Circulating Water / P-2308 A/B discharge NaOH, wt-% UOP 209 1/D 1/D
pH Occas. Occas.
SC-2312 / 21 023-PID-0021-030 DIH Overhead / 023-FV-034 Composition, wt-% UOP 551 1/D 3/D
MON-clear ASTP D 2700 Occas. Occas.
SC-2313 / 1B 023-PID-0021-028 DIH Bottoms / 023-FV-028 Composition, wt-% UOP 551 1/D 3/D
SC-2314 / 1B 023-PID-0021-027 DIH Sidedraw / 023-FV-030 Composition, wt-% UOP 551 1/D 3/D
SC-2315 / 3B 023-PID-0021-029 DIH Combined Product, Overhead Plus Bottoms / Composition, wt-% UOP 551 1/D 3/D
Outlet E-2318 Total Chlorides, wt-ppm UOP 395 Occas. 1/D
SC-2316 / 6 023-PID-0021-010 Makeup Gas from Methanator Zinc Oxide Bed / Composition, mol-% UOP 539 Occas. Occas.
R-2301 Total Sulfur, mol-ppm UOP 212 or 1/W 1/D
Draeger Tube
CO/CO2, mol-ppm UOP 603 Occas. Occas.
3.1 GENERAL
The "Test Method" column in Table 1 presents the methods recommended for the test.
The methods represent, in UOP's opinion, the best methods for the analysis from an
accuracy, precision, convenience and speed point of view. Cost of special equipment
was also considered for the methods. Alternative methods may be substituted if the test
method is not specified in the guarantee agreements.
The tests labeled UOP are UOP methods. The ASTM procedures given in the table can
be found in the Annual Book of ASTM Standards, Section 5, Volumes 5.01, 5.02, 5.03
and 5.04 and Section 6, Volume 6.03.
Samples should be taken on a regularly scheduled basis by authorized personnel
knowledgeable in the procedure.
Operator equipment required during sampling includes rubber gloves and protective face
shields.
For gas samples 500 ml stainless steel sample cylinders are preferred.
For all liquid samples, 1000 ml stainless steel sample cylinders are preferred. Sample
cylinders should be received from the laboratory properly cleaned. Cylinders should have
the pressure ratings stamped on them.
All samples leaving the process area for the laboratory should be tagged with the
following information: sample description, sample source, analyses requested, date and
time sampled.
3.2 SAMPLES FOR UOP ANALYSIS

Samples which are sent to UOP for analysis sometimes go astray, either in shipping or
within UOP. In order to minimize delays caused by lost, misplaced, or unidentified
samples, please observe the following procedures:
1. Determine the sample size required by consulting the UOP Service Department.
2. Identify each sample with refinery name, location, unit name, sample identification,
date sampled, and analyses requested. Make certain that the sample tag is well
secured to the sample and remains legible, even if it is wet with water or the
hydrocarbon.
3. When shipping samples, mail or phone shipping information (airway bill, flight
number, bill of loading, etc.) to UOP.
4. Send a copy of the request for analysis with the samples; send the original to:
Light Ends Processing Group
UOP Technical Service Department
25 E. Algonquin Road
USA
5. Ship samples to:
UOP Research Center
Central Receiving
50 E. Algonquin Road

USA
Attention: Sample Receiving
6. If the sample is flammable or toxic, label the container appropriately and ensure that
all government and shipper safety requirements are met.
7. We recommend that non-hazardous samples be shipped by mail or courier, and
hazardous samples be shipped by Burlington Air or Emery Worldwide. All samples
must be shipped via O'Hare International Airport, Chicago, Illinois, USA. Mark the
outside of the carton 'CLEAR THROUGH CIRCLE INTERNATIONAL".
8. The samples must be classified for "IATA" regulations if shipped by air, or "IMO"
regulations if shipped by sea.
9. The sample shipment MUST have a Customs invoice (sometimes referred to as the
Pro Forma invoice), see attached example. Failure to send samples with proper
documentation will result in a delay clearing customs. Pro Forma invoice
requirements vary depending on the country of origin, however the basic information
required is:
Quantity of Sample
Identification/Description of Sample (including Material Safety Datasheet - MSDS)
Statement of value for customs purposes only
The customs invoice should also indicate "TSCA exempt samples for R&D purposes".
(This refers to the Toxic Substances Control Act, which requires identification of
chemicals imported into the USA for commercial purposes. Samples for Research
and Development or characterization are exempt if so declared.)
A copy of the invoice should be faxed to the UOP Traffic Department at (847) 391-
2097.
10. Include a copy of the attached Form with the samples.
11. Hand carrying of samples to UOP without the documentation described above is
illegal. Therefore, UOP employees and customers are to refrain from transporting any
samples by this method, from any refinery to any UOP laboratory or office.
3.3 SAMPLE CONTAMINATION - CONTAINER PROBLEMS

There have been found to be problems associated with the shipment of liquid samples
shipped in standard laboratory vials with conical polyethylene caps. It has been found,
through controlled tests, that samples cannot only permeate out of the containers in
question, but that the samples can actually cross permeate between samples.
Tests were performed with the type of vials generally available in the laboratory using caps
with liners of various materials. In a typical test, a vial containing only benzene and a vial
containing only orthoxylene were placed together in a sealed jar for a period of time. The
jars were heated to 40°C (a very possible shipping temperature) to speed the
permeation. Tests were done both with the vials in an upright position and with the vials
lying on their side so that the liquid would contact the caps. The common conical
polyethylene lined caps cross-permeated from 0.50 to 4.0% under these conditions.
Paper lined caps produced terrible results. Corks and Teflon linings worked well until
they were tipped over, at which point these containers also produced terrible results. The
best caps found thus far are the foil lined caps. The aluminum foil lined caps cross-
permeate only slightly and the tin foil lined caps do not cross-permeate at all.
The following recommendations are made: If possible, keep the samples cool.
Temperature does affect the permeation rate through some materials. Use tin foil lined
caps when available and keep the samples as far apart as possible so they will have less
tendency to cross-permeate.
3.4 MINIMUM SAMPLE SIZE IF SENT TO UOP FOR ANALYSIS

Analyses Preferred minimum (cm3)
Density 100
Distillation 210(1)
Composition 50
Sulfur, Microcoulometric 10
Nickel Reduction 100
Nitrogen, Kjeldahl 800
Microcoulometric 10
Chloride 100
Arsenic 400
Lead 100
Product
Density 100
Distillation 210(1)
Composition by GC 150
All Common Analyses 2 liters
Note: (1) May also be used for density.

Table 2 - Penex Streams Contamination Limits and Performance Identifiers
Contamination Units /
Stream Test Performance Identifiers
Liquid Feed Total Sulfur Target <0,1 ppm (0,5 wppm MAX.)
Total Nitrogen Target <0,1 ppm (0,5 wppm MAX.)
Water 0,0 ppm (0,1 ppm MAX.)
Oxygen and Oxygen Nil. (Less than the lowest detectable limits)
Compounds, Methanol,
Carbonyl
Arsenic 1 ppb (Less than the lowest detectable limits)
Lead 10 ppb (Less than the lowest detectable limits)
Copper <20 ppb (Less than the lowest detectable limits)
Fluoride <0,5 ppm (Less than the lowest detectable limits)
Other Metals: Iron, Sodium Nil. (Less than the lowest detectable limits)
Makeup Gas Composition (by GC) Sufficient H2 so outlet H2/HC can be maintained
above 0,05 mol/mol. (Usually >70% H2)
Basic Nitrogen Target <0,01 ppm (0,5 ppm MAX.)
Water 0,0 ppm (0,1 ppm MAX.)
Oxygen and Oxygen CO + CO2 <10 ppm (Less than lowest detectable
Compounds limits) CO <1 ppm
H2S (by Draeger) Target <0,01 ppm (1,0 ppm MAX.)
Lead Reactor Effluent Composition (by GC) iC 5

iC 5 + nC5
Composition (by GC) no benzene
Stabilizer Off-Gas Composition (by GC) low C5+, minimize C4's

H2S (by Draeger) 0,0 ppm (Less than lowest detectable limits)
Caustic Scrubber HCl 0,0 ppm (Less than lowest detectable limits)
Off-Gas
Contamination Units /
Stream Test Performance Identifiers
Stabilizer Bottoms Composition (by GC) No C3-
iC 5
=> 70%
iC 5 + nC 5
2 − 2 DMB
= 30 − 35%
C6 P
2 − 3 DMB
= 10%
C6 P
2 MP
= 30%
C6 P
3 MP
= 16%
C6 P
nC 6
= 9 − 12%
C6 P
MCP
= 50%
MCP + CH
C6 Ring Opening = 40%
Total Chloride, HCl <1.0 ppm (Less than the lowest detectable limits)
Scrubber Circulating Composition (by titration) 10wt-% to 2 wt-% NaOH

Caustic
Visual Inspection Not excessively graying
4. ON LINE ANALYSERS
Analysers located in the Penex / DIH unit are the following:
Item PID ref. Datasheet ref. Analysis

023-AI-002 8474L-023-PID-0021-017
8474L-023-PDS-AE-001 Hydrogen Process Analyser
023-AI-003 8474L-023-PID-0021-022
023-AI-001 A 8474L-023-PID-0021-011
023-AI-001 B 8474L-023-PID-0021-013 8474L-023-PDS-AE-002 Moisture Analyser
023-AI-001 D 8474L-023-PID-0021-019
023-AI-004 8474L-023-PID-0021-027
8474L-023-PDS-AE-003 Process Gas Chromatograph
023-AI-005 8474L-023-PID-0021-030
Supplied by Package
023-AI-006 8474L-023-PID-0021-031 Vendor pH Analyser
8474L-023-PDS-AE-004
UNIT ISOM (023) Page : 1/ 1
13 PROCESS CONTROL
13.1 DISTRIBUTED SYSTEM CONTROL (DCS)
The text will be prepared by JVD instrument manager for all OCs
CHAPTER 14
DRAWINGS
CONTENTS
1 PLOT PLAN AND HAZARDOUS CLASSIFICATION
2 PROCESS FLOW DIAGRAMS AND MATERIAL SELECTION DIAGRAMS
3 PIPING AND INSTRUMENTATION DIAGRAMS
4 OTHER DRAWINGS
1 PLOT PLAN AND HAZARDOUS CLASSIFICATION

Refer to the following documents:
8474L-012-DW-0051-001 Plot Plan – NHT / CCR / ISOM

8474L-012-DW-1920-001 Hazardous Area Classification Plan – NHT / CCR
/ ISOM
2 PROCESS FLOW DIAGRAMS AND MATERIAL SELECTION DIAGRAMS

8474L-023-MSD-0011-001 Makeup Gas Station
8474L-023-MSD-0011-002 Feed And Regeneration Section
8474L-023-MSD-0011-003 Reactor Section
8474L-023-MSD-0011-004 Stabilizer And Net Gas Scrubber Section
8474L-023-MSD-0011-005 Deisohexanizer Section
8474L-023-PFD-0010-001 Makeup Gas Section
8474L-023-PFD-0010-002 Feed And Regeneration Section
8474L-023-PFD-0010-003 Reactor Section
8474L-023-PFD-0010-004 Stabilizer And Net Gas Scrubber Section
8474L-023-PFD-0010-005 Deisohexaniser Section
8474L-023-PFD-0010-006 Material Balance Sheet
3 PIPING AND INSTRUMENTATION DIAGRAMS

8474L-023-PID-0021-010 Methanator
8474L-023-PID-0021-011 Makeup Gas Driers
8474L-023-PID-0021-012 Regenerant Vaporizer/Superheater
8474L-023-PID-0021-013 Feed Driers
8474L-023-PID-0021-014 Bleeder Knockout Drum
8474L-023-PID-0021-015 Feed Surge Drum
8474L-023-PID-0021-016 Chloride Injection
8474L-023-PID-0021-017 Cold Combined Feed Exchanger
8474L-023-PID-0021-018 Hot Combined Feed Exchanger And Charge Heater
8474L-023-PID-0021-019 Reactors
8474L-023-PID-0021-020 Stabilizer
8474L-023-PID-0021-021 Stabilizer Receiver
8474L-023-PID-0021-022 Net Gas Scrubber
8474L-023-PID-0021-023 Caustic Circulation And Dilution
8474L-023-PID-0021-024 Caustic Dilution
8474L-023-PID-0021-025 Caustic Degassing Drum
8474L-023-PID-0021-026 Deisohexanizer
8474L-023-PID-0021-027 Deisohexanizer Bottoms And Side Draw
8474L-023-PID-0021-028 Deisohexanizer Bottoms And Side Draw
8474L-023-PID-0021-029 Deisohexanizer Upper Side Draw And Isomerate Product
8474L-023-PID-0021-030 Deisohexanizer Receiver
8474L-023-PID-0021-031 Spent Caustic Neutralization
8474L-023-PID-0021-032 PID Interlock Details
8474L-023-PID-0021-050 E-2310/E-2313 Air Cooler Details
8474L-023-PID-0021-051 E-2317 Air Cooler Details
8474L-023-PID-0021-060 Sample Connection Details
8474L-023-PID-0021-070 Penex Level Connection Details
8474L-023-PID-0021-071 Penex Level Connection Typicals
8474L-023-PID-0041-090 Penex Pump Auxiliaries Details
8474L-023-PID-0041-091 Penex Pump P-2311 A/B - Auxiliaries Details
8474L-023-PID-0090-001 Symbology - Typicals For On/Off Valves
8474L-012-PID-0031-901 Flare and Fuel Gas
8474L-012-PID-0031-902 Flare And Fuel Gas
8474L-012-PID-0031-911 Closed Drain Collection
8474L-012-PID-0031-921 HP MP & LP Steam
8474L-012-PID-0031-931 Cooling Water Service Water and Potable Water
8474L-012-PID-0031-941 Plant Air Instrument Air & Nitrogen

8474L-012-PID-0031-945 Boiler Feed Water & Condensate Header
8474L-012-PID-0031-946 Boiler Feed Water & Condensate Header
8474L-012-PID-0031-951 Caustic
8474L-012-PID-0031-955 Closed Drain System
8474L-012-PID-0031-961 Utility Distribution - Oily Water System
8474L-012-PID-0031-965 Utility Distribution - Oily Mist System
8474L-012-PID-0031-990 Battery Limit
8474L-200-A0103-4046-001-431 Piping and Instrument Diagram X-2302
8474L-200-A0103-4046-001-481 Piping and Instrument Diagram X-2304
4 OTHER DRAWINGS
Electric single line diagram
Underground sewer network
Fire fighting water distribution diagram

Dung Quat Refinery Light Naphta Isomerization Unit

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PROCESS DATA SHEET

Project N° - Unit Doc. type Equipment N° Serial N° Rev. index

LOCATION DUNG QUAT PENEX UNIT (023)

A 27-JUL-07 C. VERDON J-P. BINET R. LEFEBVRE ISSUE FOR REVIEW

DUNG QUAT REFINERY

CHAPTER 1 BASIS OF DESIGN

CHAPTER 2 PROCESS DESCRIPTION

CHAPTER 3 DESCRIPTION OF UNIT CONTROL

CHAPTER 4 UILITY, CHEMICAL AND CATALYST REQUIREMENTS

CHAPTER 5 PREPARATION FOR INITIAL START-UP

CHAPTER 6 INITIAL AND NORMAL START-UP

CHAPTER 7 NORMAL SHUTDOWN

2. CATALYST UNLOADING AND HANDLING PROCEDURES

CHAPTER 8 EMERGENCY SHUTDOWN PROCEDURES

CHAPTER 9 SAFETY EQUIPMENT AND PROCEDURES

CHAPTER 10 INSTRUMENT DATA

CHAPTER 11 SUMMARY OF MAJOR EQUIPMENT

CHAPTER 13 PROCESS CONTROL

1. DUTY OF THE PLANT

1.2 FUNCTION OF THE UNIT

2.1 AIR TEMPERATURE

2.2 RELATIVE HUMIDITY

2.5 AIR BAROMETRIC PRESSURE

2.8 MISCELLANEOUS DATA

3. FEEDSTOCKS AND PRODUCTS SPECIFICATIONS

3.1 FEEDS CHARACTERISTICS

3.2 PRODUCTS SPECIFICATIONS

4. OVERALL MATERIAL BALANCE OF THE UNIT

4.1 PROCESS INLET

4.2 PROCESS OUTLET

5. BATTERY LIMIT CONDITIONS

5.1 FEEDSTOCKS BATTERY LIMIT CONDITIONS

5.2 PRODUCTS BATTERY LIMIT CONDITIONS

5.3 UTILITIES BATTERY LIMIT CONDITIONS

6.1 EQUIPMENT OUTSIDE LICENSOR SCOPE

6.2 MANDATORY SUPPLY

7. GAS AND LIQUID EFFLUENTS

1. DUTY OF THE PLANT

1.2 FUNCTION OF THE UNIT

Light naphtha from unit 012 Isomerate to TK-5106 A/B

20°Be Caustic from unit 039

Service water PENEX / DIH Flare to unit 057

2.1 AIR TEMPERATURE

Direction % of time for each Quadrant

e. Exposure to conductive or corrosive dusts (carbon, iron oxide, ammonium nitrates or

3. FEEDSTOCKS AND PRODUCTS SPECIFICATIONS

3.1 FEEDS CHARACTERISTICS

3.1.1 HYDROTREATED LIGHT NAPHTHA

Feed rate = 6500 BPSD.

Property Value Test Method

Total C5, wt. % 30.5 min.

3.1.2 MAKEUP GAS

The composition of hydrogen is the following in normal operation:

3.2 PRODUCTS SPECIFICATIONS

C5+ Product Yield at Start-of-Run, 95.2

Design Case Alternate Case

3.2.2 NET GAS

Design Case Alternate Case

4. OVERALL MATERIAL BALANCE OF THE UNIT

4.1 PROCESS INLET

Design Case Alternate Case

4.2 PROCESS OUTLET

Design Case Alternate Case