R2B-P3-206-02-A-FO-00001 - Rev.1 - Operation Philosophy - Eng

PHASE II OF REFINERY IN DOS
BOCAS (FCC)
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Doc. TITLE Operation Philosophy
Rev. 1
PTI-ID-O-004-2-
Contract Doc. No. R2B-P3-206-02-A-FO-00001 Contract No.
2020
Contractor
Contractor Doc. No. SO6625-ES0B-PHL-P3206002 Job. No.
SO6625
Operation Philosophy
FCC
BETWEEN
PTI-Infraestructura de Desarrollo, S.A. de C.V.
AND
Samsung Ingeniería Manzanillo, S.A. de C.V. /

Asociados Constructores DBNR, S.A. de C.V.
“COMPLEMENTARY ENGINEERING, PROCUREMENT, CONSTRUCTION AND SUPPORT DURING

TESTS AND STARTUP OF THE CATALYTIC CRACKING FCC PLANT FOR THE REFINERY IN DOS
BOCAS, PARAÍSO, TABASCO” (PHASE II)
Contract No. PTI-ID-O-004-2-2020
1 27 AUG 21 ISSUE FOR CONSTRUCTION JG Jung YD Cho KH Lee
0 22 APR 2020 Issue for Cost Estimation JG Jung YD Cho KH Lee
A 27 MAR 20 ISSUE FOR REVIEW JG Jung YD Cho KH Lee
Rev. Date Description Prepared by Reviewed by Approved by
This document, including any patented or patentable features, embodies confidential information of Samsung Ingeniería Manzanillo, S.A. de
C.V. and its use is conditioned upon the user’s agreement not to reproduce the document in whole or in part. Nor the material described thereon
nor to use the document for any purpose other than specifically permitted in writing by Samsung Ingeniería Manzanillo, S.A. de. C.V.
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REVISION HISTORY
Rev DATE DESCRIPTION
A 27 MAR 20 Issue for Review
0 22 APR 2020 Issue for Cost Estimation
ISSUE FOR CONSTRUCTION

1 27 AUG 21
-Special operating consideration section is added.
* Notes:
This page records all revisions on the procedures
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TABLE OF CONTENTS
1. GENERAL ................................................................................................... 10
1.1 INTRODUCTION ................................................................................... 10
2. RX-REGEN and MAIN COLUMN ................................................................ 11
2.1 INTRODUCTION ................................................................................... 11
2.1.1 PROJECT BACKGROUND ................................................................... 11
2.1.2 PROJECT SCOPE ................................................................................ 11
2.1.3 OPERATING CONDITION SUMMARY........................................... 12
2.1.4 PROCESS DESCRIPTION ............................................................. 13
2.1.5 FCC FEED STOCKS ...................................................................... 13
2.1.6 FCC PRODUCTS ........................................................................... 14
2.2 PROCESS VARIABLES ........................................................................ 16
2.2.1 REACTOR (DC-21001) ................................................................... 16
2.2.1.1 Catalyst Management ........................................................ 16
2.2.1.2 Catalyst/Oil Ratio................................................................ 17
2.2.1.3 Charge Rate ....................................................................... 17
2.2.1.4 Combined Feed Temperature ............................................ 18
2.2.1.5 Reactor Pressure ............................................................... 18
2.2.1.6 Reactor Temperature ......................................................... 19
2.2.1.7 Recycle Rate ...................................................................... 19
2.2.1.8 Lift Gas System .................................................................. 20
2.2.1.9 Riser Steam ....................................................................... 20
2.2.1.10 Stripping Steam Rate ......................................................... 21
2.2.2 REGENERATOR (DC-21002)......................................................... 22
2.2.2.1 Air Distribution .................................................................... 22
2.2.2.2 Catalyst Condition .............................................................. 22
2.2.2.3 Coke Combustion ............................................................... 23
2.2.2.4 Combustion Air Rate .......................................................... 24
2.2.2.5 Dense Phase Temperature ................................................ 24
2.2.2.6 Recirculation Catalyst Rate ................................................ 25
2.2.2.7 Regenerator Level .............................................................. 25
2.2.2.8 Regenerator Pressure ........................................................ 26
2.2.2.9 Torch Oil............................................................................. 26
2.2.3 CHARGE PROPERTIES................................................................. 27
2.2.3.1 Boiling Range ..................................................................... 27
2.2.3.2 Carbon Residue ................................................................. 28
2.2.3.3 Characterization Factor – UOP K ....................................... 28
2.2.3.4 Color................................................................................... 29
2.2.3.5 Gravity ................................................................................ 29
2.2.3.6 Metals................................................................................. 29
2.2.3.7 Nitrogen .............................................................................. 30
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2.2.3.8 Oxygen ............................................................................... 31

2.2.3.9 Sulfur .................................................................................. 31
2.3 PROCESS FLOW AND CONTROL ...................................................... 32
2.3.1 PROCESS FLOW ........................................................................... 32
2.3.1.1 Reactor-Regenerator Section ............................................. 32
2.3.1.2 Fractionation Section.......................................................... 35
2.3.2 PROCESS CONTROL .................................................................... 38
2.3.2.1 Raw Oil Charge System ..................................................... 38
2.3.2.2 Optimix Feed Distributor Control ........................................ 40
2.3.2.3 FCC Catalyst Section – Reactor ........................................ 43
2.3.2.4 FCC Catalyst Section – Regenerator ................................. 46
2.3.2.5 Direct Fired Air Heater (DFAH) (BA-21001) ....................... 53
2.3.2.6 Fractionation Section.......................................................... 54
2.4 TROUBLESHOOTING .......................................................................... 64
2.4.2 FCC MAIN COLUMN BOTTOMS SYSTEM FOULING ................... 64
2.4.3 CATALYST LOSS ........................................................................... 66
2.5 SPECIAL PROCEDURES ..................................................................... 69
2.5.2 CATALYST SAMPLING .................................................................. 69
2.5.3 BLASTING CATALYST STANDPIPES ........................................... 70
2.5.4 DIRECT FIRED AIR HEATER ........................................................ 71
2.5.5 FLUSHING SYSTEM ...................................................................... 74
2.5.6 REACTOR VAPOR LINE BLIND .................................................... 74
2.5.7 OPTIMIX FEED DISTRIBUTOR BALANCING ................................ 77
2.5.8 CATALYST ADDITION SYSTEM.................................................... 78
2.5.9 CONTINUOUS CATALYST WITHDRAWAL SYSTEM ................... 79
2.5.10 MAIN COLUMN BOTTOMS OPTIMIZATION ................................. 81
2.6 ANALYTICAL CONTROL PROCEDURE .............................................. 85
2.7 OPERATING RECOMMENDATIONS FOR SHUTDOWNS, RESTARTS
AND EMERGENCIES ....................................................................................... 86
3. GAS CONCENTRATION ............................................................................. 87
3.1 INTRODUCTION ................................................................................... 87
3.1.1 GENERAL ....................................................................................... 87
3.1.2 PROCESS DESCRIPTION ............................................................. 88
3.2 PROCESS VARIABLES ........................................................................ 91
3.2.1 LEAN OIL FLOW TO THE ABSORBERS ....................................... 92
3.2.1.1 Primary Absorber (DA-21201) ............................................ 92
3.2.1.2 Sponge Absorber (DA-21202) ............................................ 92
3.2.2 PRIMARY ABSORBER TEMPERATURE ....................................... 92
3.2.3 HIGH PRESSURE RECEIVER TEMPERATURE ........................... 93
3.2.4 STRIPPER VAPOR RATE .............................................................. 93
3.2.5 SYSTEM PRESSURE..................................................................... 93
3.2.6 OPERATING VARIABLES .............................................................. 93
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3.3 PROCESS FLOW AND CONTROL ...................................................... 96

3.3.1 RECOVERY SECTION ................................................................... 96
3.3.2 WATER WASH SYSTEM.............................................................. 102
3.3.3 FRACTIONATION SECTION ........................................................ 103
3.4 TROUBLESHOOTING ........................................................................ 105
3.5 SPECIAL PROCEDURES ................................................................... 106
3.6 ANALYTICAL CONTROL PROCEDURE ............................................ 107
AND EMERGENCIES ..................................................................................... 108
4. CAUSTIC MEROX AMINE SECTION ....................................................... 109
4.1 INTRODUCTION ................................................................................. 109
4.1.1 GENERAL ..................................................................................... 109
4.2 PROCESS VARIABLES ...................................................................... 112
4.2.1 ABSORPTION .............................................................................. 112
4.2.1.1 Low Absorber Operating Temperature ............................. 112
4.2.1.2 Amine Acid Gas Loading .................................................. 112
4.2.1.3 Amine Solution Concentration .......................................... 113
4.2.2 REGENERATION ......................................................................... 114
1. Temperature ................................................................................. 114
2. Low Pressure ................................................................................ 115
3. Low H2S Partial Pressure.............................................................. 115
4. Proper Amine Concentration ......................................................... 115
4.2.3 FEED QUALITY AND RATE ......................................................... 116
4.3 PROCESS FLOW AND CONTROL .................................................... 118
4.3.1 FUEL GAS PURIFICATION .......................................................... 119
4.3.2 LPG PURIFICATION .................................................................... 119
4.3.3 AMINE CIRCULATION ................................................................. 120
4.3.4 ACID GAS SEPARATION ............................................................. 121
4.3.5 AMINE STORAGE AND TRANSFER ........................................... 122
4.4.1 DIRTY AMINE ............................................................................... 124
4.4.2 FOAMING ..................................................................................... 127
4.4.3 FAILURE TO MEET DESIGN SPECIFICATIONS ........................ 130
4.4.4 CORROSION ................................................................................ 134
4.4.5 AMINE LOSSES ........................................................................... 137
4.5.1 LEAK TEST INSTRUCTIONS ....................................................... 140
4.5.2 MEA RECLAIMING ....................................................................... 142
4.5.2.1 BACKGROUND................................................................ 142
4.5.2.2 PROCESS FLOW ............................................................ 143
4.5.2.3 RECLAIMER OPERATIONS ............................................ 144
4.5.3 CHARGING THE SOLVENT ......................................................... 149
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4.5.4 HYDROCARBON SKIMMING....................................................... 149

4.5.4.1 Absorber........................................................................... 150
4.5.4.2 Rich Amine Flash Drum ................................................... 150
4.5.5 ANTIFOAM ADDITION ................................................................. 150
4.5.6 CARBON BED MAINTENANCE ................................................... 152
1. De-aerating ................................................................................... 152
5. Loading ......................................................................................... 153
6. De-Fining ...................................................................................... 153
7. Discharging ................................................................................... 156
AND EMERGENCIES ..................................................................................... 158
5. CAUSTIC MEROX LIQUID/LIQUID EXTRACTION .................................. 159
5.1 INTRODUCTION ................................................................................. 159
5.1.1 MEROX PROCESS OVERVIEW .................................................. 159
5.1.2 MEROX ADVANTAGES ............................................................... 161
5.1.3 HISTORY OF THE UOP MEROX PROCESS............................... 161
5.1.4 GENERAL TREATING TERMS .................................................... 165
5.1.5 CHEMICAL ABBREVIATIONS AND SYMBOLS ........................... 168
5.2.1 CATALYST CONNENTRATION ................................................... 170
5.2.2 OXYGEN INJECTION ................................................................... 170
5.2.3 ALKALINITY.................................................................................. 170
5.2.4 CONTACT..................................................................................... 171
5.2.5 HEAT (TEMPERATURE) .............................................................. 174
5.3.1 PROCESS FLOW ......................................................................... 175
1. Pretreatment ................................................................................. 179
6. Extraction Section ......................................................................... 179
5.3.2 CONTROL PHILOSOPHY ............................................................ 180
5.4.1 EXTRACTION ............................................................................... 182
5.5.1 SAND FILTER BACKWASHING ................................................... 183
5.5.2 LEAK TEST INSTRUCTIONS ....................................................... 183
5.5.3 BATCH PREWASH CAUSTIC CHANGE OUT INSTRODUCTIONS
USING FRESH CAUSTIC ........................................................................ 184
5.5.4 PREWASH CAUSTIC CHANGEOUT INSTRUCTIONS USING
REGENERATED CAUSTIC ..................................................................... 186
5.5.5 ENHANCES PREWASH BATCH COS SOLVENT CHANGE OUT
187
5.5.6 PREWASH CAUSTIC CHANGE OUT INSTRUCTIONS USING
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REGENERATED CAUSTIC ..................................................................... 188

5.5.7 EXTRACTOR LEVEL REPLENISHMENT WITH FRESH CAUSTIC:
191
5.5.8 SAND FILTER LOADING INSTRUCTIONS .................................. 192
5.5.9 SAND FILTER UNLOADING PRECAUTIONS.............................. 192
AND EMERGENCIES ..................................................................................... 194
6. CAUSTIC MEROX COVENTIONAL REGENERATION ............................ 195
6.1 INTRODUCTION ................................................................................. 195
6.1.1 MEROX PROCESS OVERVIEW .................................................. 195
6.1.2 MEROX ADVANTAGES ............................................................... 196
6.1.3 HISTORY OF THE UOP MEROX PROCESS............................... 197
6.1.4 GENERAL TREATING TERMS .................................................... 201
6.1.5 CHEMICAL ABBREVIATIONS AND SYMBOLS ........................... 204
6.2.1 CATALYST CONCENTRATION ................................................... 206
6.2.2 OXYGEN INJECTION ................................................................... 207
6.2.3 ALKALINITY.................................................................................. 210
6.2.4 CONTACT..................................................................................... 210
6.2.5 HEAT (TEMPERATURE) .............................................................. 212
6.3.1 PROCESS FLOW OVERVIEW ..................................................... 214
1. Regeneration Section ................................................................... 215
6.3.2 CONTROL PHILOSOPHY ............................................................ 220
6.4.1 REGENERATION ......................................................................... 223
6.4.2 OTHER TOOLS TO CHECK HE CAUSTIC REGENERATION
SECTION ................................................................................................. 225
6.4.2.1 Shake Test ....................................................................... 225
6.4.2.2 Disulfide Separator Vent Gas ........................................... 225
6.4.3 DISULFIDE SEPARATION ........................................................... 226
6.4.4 EMULSIFICATION AND CAUSTIC ENTRAINMENT .................... 226
6.5.1 DISULFIDE SAND FILTER BACKWASHING ............................... 227
6.5.2 OXIDIZER LOADING INSTRUCTIONS ........................................ 227
6.5.3 OXIDIZER UNLOADING PRECAUTIONS .................................... 228
6.5.4 DISULFIDE SEPARATOR LOADING INSTRUCTIONS ............... 228
6.5.5 DISULFIDE SEPARATOR UNLOADING PRECAUTIONS ........... 230
6.5.6 VENT TANK LOADING INSTRUCTIONS ..................................... 230
6.5.7 VENT TANK UNLOADING PRECAUTIONS ................................. 231
6.5.8 DISULFIDE SAND FILTER LOADING INSTRUCTIONS .............. 231
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6.5.9 DISULFIDE SAND FILTER UNLOADING PRECAUTIONS .......... 232

6.5.10 DISULFIDE SCRUBBER LOADING INSTRUCTIONS ................. 232
6.5.11 DISULFIDE SCRUBBER UNLOADING PRECAUTIONS ............. 233
AND EMERGENCIES ..................................................................................... 235
7. PROPYLENE RECOVERY UNIT .............................................................. 236
7.1 INTRODUCTION ................................................................................. 236
7.1.1 SCOPE ......................................................................................... 236
7.1.2 PURPOSE .................................................................................... 236
7.1.3 BLOCK FLOW DIAGRAM ............................................................. 238
7.2.1 PRU PROCESS VARIABLES ....................................................... 240
7.2.1.1 Feed Quality ..................................................................... 240
7.2.1.2 Feed Rate ........................................................................ 240
7.2.1.3 C3/C4 Split ......................................................................... 240
7.2.1.4 Deethanizer Product Quality ............................................ 240
7.2.1.5 Propylene Purity ............................................................... 241
7.2.2 FRACTIONATOR PROCESS VARIABLES .................................. 241
7.2.2.1 Material Balance............................................................... 241
7.2.2.2 Heat Balance .................................................................... 241
7.2.2.3 Product Control ................................................................ 242
7.3.1 C3/C4 SPLITTER (DF-21401) ........................................................ 244
7.3.1.1 Heat Input ......................................................................... 244
7.3.1.2 Reflux Rate....................................................................... 245
7.3.1.3 Overhead Pressure Control.............................................. 245
7.3.2 DEETHANIZER (DF-21402) ......................................................... 246
7.3.3 C3 SPLITTER (DF-21403) ............................................................. 247
7.3.3.1 C3 Splitter Flows ............................................................... 247
7.3.3.2 C3 Splitter Controls ........................................................... 249
7.3.4 PROPYLENE DRIERS ................................................................. 252
7.3.5 PROPYLENE TREATERS ............................................................ 252
7.4.1 PRODUCT PURITY ...................................................................... 259
7.4.1.1 Propane............................................................................ 259
7.4.1.2 Light Ends (C2 and lighter) ................................................ 259
7.4.1.3 Heavy Material (C4‘s) ........................................................ 259
7.4.2 NON-CONDENSIBLES ................................................................. 260
7.4.2.1 C3/C4 Splitter (DF-21401) ............................................... 260
7.4.2.2 C3 Splitter (DF-21402) ...................................................... 260
7.4.3 PRODUCT IMPURITIES ............................................................... 260
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7.4.3.1 Performance of the Driers ................................................ 260

7.4.3.2 Performance of the Treaters ............................................ 260
7.5.1 PROPYLENE DRIER REGENERATION ...................................... 262
7.5.2 PROPYLENE COS TREATER TEGENERATION ........................ 274
AND EMERGENCIES ..................................................................................... 289
8. SPECIAL OPERATING CONSIDERATION .............................................. 290
8.1 HP/LP Flare KO Drum (FA-21607, FA-21608) .................................... 290
8.2 Slop drain drum (FA-21606) ................................................................ 290
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1. GENERAL
1.1 INTRODUCTION
The Fluid Catalyst Cracking Unit (FCC), based on UOP process, is to be built in the
New Refinery at Dos Bocas Paraiso, Tabasco, Mexico for PTI-ID.
The objective of the unit is to convert heavy crude oil fractions into lighter, more
valuable hydrocarbon products at high temperature and moderate pressure in the
presence of a finely divided silica / alumina based catalyst, and to produce light
hydrocarbon gases (C2-) which are normally used within the refinery as fuel gas, LPG
olefins and paraffins, gasoline, light cycle oil (LCO), and clarified oil (CLO, sometimes
referred to as main column bottoms).
The FCC Unit is designed for;

Design Capacity = 94,000 BPSD of fresh hydro-treated Vacuum Gas Oil Feed
Maximum Capacity = 110% of design capacity
Short-term turndown (50% of hydraulic turndown) = 47,000 BPSD
Expected on-stream factor = 97%
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2. RX-REGEN and MAIN COLUMN

2.1 INTRODUCTION
2.1.1 PROJECT BACKGROUND
The PEMEX Dos Bocas FCC Unit is to be revamped to process 94,000 BPD feed. The
basis for the operation is UOP Yield Estimate # 5325.
2.1.2 PROJECT SCOPE

The modifications for this revamp within UOP’s scope are:
Reactor Side (DC-21001)

• VSS G3 Reactor
• Optimix
• Stripper Packing
• Main Colum Bottom Recycle to Riser
• Naphtha quench to riser for startup
Regenerator Side (DC-21002)

• Combustor (BA-21001)
• Flue Gas Cooler (SPE-21012)
• Orifice Chamber (FA-21006)
• Diverter Valve System (SPE-21014)
• Electrostatic Precipitator (SPE-21013)
• Bypass Stack (SPE-21017, SPE-21019)
• Main Air Blower Compressor (GB-21001)
Main Column (DF-21101)

• Main Column Bottoms Stripper (DS-21101)
Bottoms Filtration System (SPE-21101)
• LCO Stripper (DS-21102)
• HCO Section
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2.1.3 OPERATING CONDITION SUMMARY
The design operating conditions of the revamped unit are shown below. Please note
that these operating conditions are for design purposes and are useful as a guide to
operations. However, the optimized processing conditions may vary somewhat from
these design conditions.
UOP Yield Estimate 5325

Raw Oil Charge Rate
BPSD 94,000
lb/hr
Raw Oil Feed Properties
Specific Gravity
° API 25.6
Molecular Weight 403
UOP K 12.04
Nickel, wppm 0.0
Vanadium, wppm 0.0
Sulfur, wt% 0.07
Conradson Carbon, wt%
Operating Conditions
Combined Feed Ratio 1.06
Oil Temperature to Riser, °F 500
Reactor Temperature, °F 998
Reactor Pressure, psig 25
Lift Steam to Riser, wt% of fresh feed 1.0
Atomizing Steam to Feed Distributors, wt% of fresh 4.0
feed
Catalyst/Oil Ratio, lb/lb 8.09
Regenerated Catalyst Temperature, °F 1303
Dry Air/Coke, lb/lb 13.45
Conversion, vol% (EP at 430°F) 84.45
Catalyst Information
MAT Activity 73.1
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2.1.4 PROCESS DESCRIPTION
The Fluid Catalytic Cracking (FCC) process converts heavy crude oil fractions into
lighter, more valuable hydrocarbon products at high temperature and moderate
pressure in the presence of a finely divided silica / alumina based catalyst. In the
course of cracking large hydrocarbon molecules into smaller molecules, a nonvolatile
carbonaceous material, commonly referred to as coke, is deposited on the catalyst.
The coke laid down on the catalyst acts to deactivate the catalytic cracking activity of
the catalyst by blocking access to the active catalytic sites. In order to regenerate the
catalytic activity of the catalyst, the coke deposited on the catalyst is burned off with
air in the regenerator vessel
One of the important advantages of fluid catalytic cracking is the ability of the catalyst
to flow easily between the reactor and the regenerator when fluidized with an
appropriate vapor phase. In FCC units the vapor phase on the reactor side is vaporized
hydrocarbon and steam, while on the regenerator side the fluidization media is air and
combustion gases. In this way, fluidization permits hot regenerated catalyst to contact
fresh feed; the hot catalyst vaporizes the liquid feed and catalytically cracks the
vaporized feed to form lighter hydrocarbon products. After the gaseous hydrocarbons
are separated from the spent catalyst, the hydrocarbon vapor is cooled and then
fractionated into the desired product streams. The separated spent catalyst flows via
steam fluidization from the reactor to the regenerator vessel where the coke is burned
off the catalyst to restore its activity. In the course of burning the coke a large amount
of heat is liberated. Most of this heat of combustion is absorbed by the regenerated
catalyst and is carried back to the reactor by the fluidized regenerated catalyst to
supply the heat required to drive the reaction side of the process. The ability to
continuously circulate fluidized catalyst between the reactor and the regenerator
allows the FCC to operate efficiently as a continuous process.
2.1.5 FCC FEED STOCKS
FCC units process heavy oil from a variety of refinery flow schemes. Generally, the
feed comes from either the refinery crude unit or vacuum unit and constitutes the
fraction of the crude boiling in the range of 650 to 1000+°F (350 to 550+°C). There
may be additional feed preparation units upstream of the FCC such as a hydrotreater
or deasphalter. Figure 1 below shows a schematic diagram of the possible refinery
flows providing feed to an FCC unit.
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Figure 1
Refinery Process Flow
In addition, FCC units commonly process heavy fractions from other conversion units
as part of the combined FCC feed blend. Examples of these types of streams are
coker gas oil and hydrocracker fractionator bottoms.
2.1.6 FCC PRODUCTS
The products obtained from the FCC are light hydrocarbon gases (C2-) which are
normally used within the refinery as fuel gas, LPG olefins and paraffins, gasoline, light
cycle oil (LCO), and clarified oil (CLO, sometimes referred to as main column bottoms).
In addition, flue gas is generated from the burning of coke in the regenerator. Heat is
recovered from the flue gas and is used to make steam. Figure 2 shows typical routes
for the FCC product streams going to further processing and ultimately to blending into
the refinery product pools.
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Figure 2
Typical Use of FCC Products
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2.2 PROCESS VARIABLES
The reactor and regenerator operate together as an integrated unit, but it is convenient
to discuss the process variables in each section independently, even though it is
impossible to make a process change in one section without affecting the other.
2.2.1 REACTOR (DC-21001)
The reactor section variables are adjusted for optimum reactor severity. A measure of
the severity is conversion, which is defined as the liquid volume percent of raw oil
charge cracked to gasoline and lighter products. The conversion should be corrected
for any gasoline contained in the raw oil, and it is conventional to correct the yield of
cracked cycle oils to that which would be produced if the 90% point of the gasoline
distillation occurred at 380°F (193°C).
Conversion and product properties change with reaction severity. Product demand is
the major consideration in selecting reaction severity. A high severity mode of
operation (approximately 85-90 LV-% conversion) will yield large amounts of LPG,
while a low severity mode (approximately 45-55 LV-% conversion) will produce more
distillate. The most common mode of operation is the gasoline mode that operates at
about 75-80 LV-% conversion. Of course, conversion and product yields are also
affected by charge stock properties.
It is important to note that gasoline yield does not always increase with reaction
severity. If severity is raised too high, overcracking will occur with the result that more
LPG will be produced at the expense of gasoline yield.
2.2.1.1 Catalyst Management
Good management of the catalyst inventory is important to a smooth operation. Fresh

catalyst must be added to the unit to maintain the desired level of activity and to make
up for physical losses. One must realize that because of the unit’s large catalyst
inventory, it will take a significant amount of time for the effects of a catalyst
replacement program to become fully apparent. Results can also be clouded by
changing feedstocks and operating conditions that affect product yields.
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Fresh catalyst addition should be made as continuously and evenly as possible.

Batchwise addition tends to affect conversion and there is evidence that increased
losses also result. It is recommended that regenerated catalyst be sent to the catalyst
supplier at least bi-weekly for analysis, and results plotted together with other process
conditions so that trends are readily observed. A program for the makeup catalyst type
and addition rate should be adhered to for a period of months before changes in
catalyst replacement are made. An accurate method for accounting for catalyst
additions and losses should be established.
Equilibrium catalyst should be withdrawn as necessary when fresh catalyst addition

results in an increase in the regenerator inventory.
2.2.1.2 Catalyst/Oil Ratio
Reference is frequently made to the catalyst/oil ratio (C/O), which is the ratio of lb/hr
(kg/hr) of catalyst circulated to lb/hr (kg/hr) of fresh feed. The catalyst/oil ratio is not an
independent variable, as it increases with an increase in reactor temperatures, and
decreases with higher regenerator or combined feed temperatures. When process
conditions are changed so that an increase in C/O occurs, an increase in conversion
and in coke yield will also be observed.
An increase in catalyst circulation at a constant reactor temperature will:
1. Increase conversion
2. Increase light gas yield
3. Increase C3 and C4 yields.
4. Decrease C3 and C4 olefinicities.
5. Increase gasoline aromatic content.
6. Decrease gasoline olefin content.
7. Increase aromatic content of the LCO.
8. Increase coke yield.
2.2.1.3 Charge Rate
The unit will accommodate quite wide variations in charge rate at constant conversion.
During turndown or when lighter feedstocks are being processed, a decrease in coke
production will cause a decrease in regenerator temperature. If the decrease in
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temperature is large enough to affect stable operation, it will be necessary to add main
column bottoms recycle to the riser to increase coke production in order to help the
unit heat balance. Charge rate is set as desired by the refiner based on the existing
economics.
2.2.1.4 Combined Feed Temperature

The combined feed temperature is adjusted through the raw oil preheat and the
recycle flow temperatures. The effect of a change in the combined feed preheat can
be predicted from the energy balance around the reactor and regenerator. An
increased preheat temperature at a constant reactor temperature will:
1. Increase conversion.
2. Increase light gas yield.
3. Increase C3 and C4 olefinicities.
4. Increase gasoline research octane number (RON).
5. Increase gasoline aromatic and olefin content.
6. Increase light cycle oil aromatic content
Although the coke production will decrease with an increase in preheat temperature,
the delta coke will increase and drive the regenerator temperature up. The delta coke
is the major variable of the two affecting the regenerator temperature.
2.2.1.5 Reactor Pressure
The pressure in the reactor is normally varied very little. There is a trade off here as a
higher reactor pressure would reduce the Gas Concentration Unit gas compressor
horsepower requirements, but it would also increase the main air blower horsepower.
Higher pressure would also reduce the required size of the vessels.
The olefin content of the products will decrease with an increase in the hydrocarbon
partial pressure. Conversion will increase somewhat. Coke laydown will increase
slightly, an effect that may be offset by adding steam or inert gas to reduce the
hydrocarbon partial pressure. This may, however, defeat the original purpose of
raising the reactor pressure.
Reactor pressure normally varies slightly with changes in feed rate and loading of the
main column. The operator has some element of control, but pressure must be kept
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within narrow limits around the design value to avoid problems with riser and cyclone
velocities. Normal first stage cyclone inlet velocities are in the 65 ft/s (20 m/s) range.
Higher velocities are better for cyclone efficiency, but worse with respect to the greater
amount of catalyst carried up to them as the vessel superficial velocity increases.
Higher velocity also increases cyclone erosion problems.
2.2.1.6 Reactor Temperature
Reactor temperature is the prime control of reactor severity. An increase in reactor

temperature at a constant catalyst circulation rate will:
1. Increase conversion.
2. Increase light gas yield.
3. Increase C3 and C4 olefinicities.
4. Increase gasoline research octane number (RON).
5. Increase gasoline aromatic and olefin content.
6. Increase light cycle oil aromatic content.
The coke yield may also increase slightly, but this will depend on other conditions as
well.
2.2.1.7 Recycle Rate
The recycle rate determines the combined feed ratio (CFR), which is defined as:
CFR = 1 + recycle feed
Where, recycle = total of recycle rates

feed = raw oil charge rate
During normal operation, recycle to the riser should not be necessary. However, during
turndown or when lighter feedstocks are being processed, it may be necessary to add
recycle to the riser to help the unit heat balance.
An increase in the recycle rate will:

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1. Increase the catalyst circulation rate.

2. Increase the coke production.
3. Increase the regenerator temperature.
4. Increase the gas make.
2.2.1.8 Lift Gas System
The lift gas plus lift steam rates are usually not varied during normal operation. An
increase in the lift gas quantity would have the following effects:
1. Increase the wet gas compressor loading.

2. Increase the main column overhead loading.
3. Increase the gas concentration unit loading.
Reduction in the amount of lift gas would decrease the hydrocarbon partial pressure
in the riser lift section and the catalyst would be subject to deactivation in the higher
steam environment. Reduction in the lift gas would also decrease the lift section
velocity as well as increase the pressure drop across the lift section. Eventually a point
would be reached where the pressure drop would increase rapidly and choke the riser,
resulting in a loss of the regenerated catalyst slide valve differential. As a minimum,
UOP does not recommend decreasing velocity below 10 ft/s (3 m/s) in the lift section
of the riser.
2.2.1.9 Riser Steam
During normal operation, riser steam consisting of a combination of lift and atomization
(primary and secondary) steams is injected into the elevated feed system. The amount
of each steam is dependent on the targeted velocities in the acceleration and mix
zones, as well as the pressure drop across the feed distributors.
Lift steam is injected into the wye section of the riser as lift media. This steam (possibly
in conjuction with lift gas) lifts the hot catalyst up the riser to the feed injection point.
An acceleration zone velocity of 12-15 feet/sec is targeted and is accomplished with
the injection of lift steam.
Primary atomization steam is injected into the distributor assembly to assist with
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atomizing the feed, flowing in the annulus between the inner and outer assembly. As
the oil and steam mix inside the top of the distributor, an additional atomization step is
provided. This improves the catalyst/oil contact as the oil is sprayed out in small
droplets. Steam also emulsifies the oil due to shear stresses created in the pressure
drop across the feed distributor. Emulsification provides better feed dispersion as the
water expands to steam in the riser. The amount of primary atomization steam is
typically 1-2.5 wt-% of the raw oil charge, depending on the feed type, more steam
being required for heavier, resid type feeds.
For heavier feeds, an additional atomization step is achieved with the use of secondary
atomization steam. The secondary atomization steam, typically 0.2 wt-% of the raw oil
charge, is injected directly into the charge to the riser feed distributor. During turndown,
for both heavier and lighter feeds, if the targeted distributor exit velocities and pressure
drop cannot be achieved via the primary atomization steam,secondary atomization
steam will either be increased or introduced. Operators should see the operating chart
created for the specific unit in question.
The total amount of riser steam, typically 2.0-3.5 wt-% of the raw oil charge will:
1. Decrease the hydrocarbon partial pressure in the riser.

2. Decrease the catalyst delta coke (weight coke/weight catalyst).
3. Decrease the regenerator temperature.
4. Decrease the light gas make.
2.2.1.10 Stripping Steam Rate
The quantity of steam required to strip the oil vapors from the spaces between the
catalyst particles is dependent upon the catalyst circulation rate. The stripping steam
rate is generally about 1.5-3.0 lb (kg) per 1000 lbs (kg) of catalyst circulated.
Alternatively, the optimum rate can be determined operationally by observing the
response of the regenerator temperature to slow stepwise decreases in the stripping
steam rate. A relatively large increase in regenerator temperature will occur when the
stripping steam rate is reduced below the minimum required and combustion of the
unstripped hydrocarbons begins. For routine operation, the steam rate should then be
increased by about 10% above this minimum. Using excessive stripping steam,
however, is detrimental as it contributes to overloading the main column overhead
system. During normal operation, stripping steam rates will need to be increased
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whenever there is a process change which results in an increase in the catalyst

circulation rate, such as:
1. An increase in the raw oil charge rate.

2. An increase in the recycle rate.
3. A decrease in the combined feed temperature.
4. An increase in the reactor temperature.
5. An increase in the catalyst cooler duty.
2.2.2 REGENERATOR (DC-21002)
The function of the regenerator is to burn the coke off the spent catalyst transferred
from the reactor. Heat generated from this combustion provides the heat necessary
for the operation of the unit. Regenerator operation influences reactor performance as
partially regenerated catalyst does not provide adequate activity for good conversion
and will affect product distribution. More important is the effect that variations in the
regenerator dense phase temperature have on the catalyst/oil ratio. A low dense
phase temperature results in high catalyst circulation which increases both the
conversion and the coke yield, but may also limit the capacity of the unit.
2.2.2.1 Air Distribution
Even air distribution is essential to good regenerator operation. If more air is passing
through one section of the bed than another, catalyst regeneration may not be
complete. Uneven temperature profiles are a sign of poor distribution. This can be
caused by a damaged distributor or operation at an air rate substantially lower than
the design air rate. Low air rates will result in grid pressure drops below design values
that can cause distributor erosion problems. Air grid distributors are normally designed
for pressure drops of 0.7-1.0 psi (0.05-0.07 kg/cm2).
2.2.2.2 Catalyst Condition
Regenerator operation is not significantly affected by normal changes in catalyst

properties. However, a substantial loss of fines from the catalyst inventory will result
in poor fluidization in the regenerator and the carbon content of the regenerated
catalyst will increase. For this reason, withdrawal of equilibrium catalyst from the
regenerator should be done regularly so that there will not be a shift of catalyst particle
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size distribution toward larger size particles. Occasionally, catalyst becomes sintered
by exposure to high temperatures, or as a result of sodium contamination. Sintering
occurs when the catalyst melts just sufficiently to close some pores. If these pores
contain coke, this coke cannot be regenerated since it is shielded from the oxygen. If
catalyst is still gray in color after laboratory regeneration in the routine carbon
determination, this color is probably due to coke trapped in sintered pores.
This indicates that the catalyst pore structure has been permanently damaged
resulting in its loss of activity.
2.2.2.3 Coke Combustion
Coke is a mixture of carbon (C) and hydrogen (H), which when burned in the
regenerator can produce carbon dioxide (CO2), carbon monoxide (CO), and water
(H2O). The carbon burning may be complete (to CO2) or it may only be partial (to a
CO and CO2 mixture). Carbon monoxide may in turn burn to CO2 and achieve
maximum combustion:
All of these reactions release heat. Complete combustion of carbon yields 14,150
Btu/lb (7863 kcal/kg) of carbon, while partial burning to CO yields only 3,960 Btu/lb
(2200 kcal/kg) of carbon. Thus, CO combustion releases roughly 72% of the total
energy available per pound of carbon. If the unit is operated for total combustion, the
maximum amount of heat is released resulting in the highest catalyst temperature.
This in turn will lower the catalyst circulation rate and the total coke production for a
given energy requirement. The catalyst will be cleaner and more active which offsets
most of the potential conversion loss because of the lower catalyst circulation. The
lower coke production also means a higher liquid yield. The high efficiency regenerator
is designed for complete CO combustion. The catalyst temperature during CO
combustion may be as high as 1300°F-1350°F (705°C- 730°C). The unit has been
designed for these extreme temperatures by using 18-8 stainless steel (Type 304H)
for all internals.
Total combustion may be initiated by using a promoted catalyst or a separate catalyst

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promoter to catalyze the conversion of CO, or in some cases by simply adding excess
air. The promoter, usually a noble metal in very small quantities, (1-2 ppm on catalyst),
preferentially burns CO to CO2 as soon as it is formed.
2.2.2.4 Combustion Air Rate
The air rate to the high efficiency regenerator should be adjusted to maintain 1-2 vol-%
excess O2 in the flue gas. If a sufficient amount of combustion air is not supplied to the
regenerator to complete the coke combustion, the regenerator will get behind in
burning. This occurs when coke is burned off the catalyst at a slower rate than it is
being formed during the cracking reaction. Partially regenerated catalyst lacks activity,
so more coke is formed on the next pass through the riser and the catalyst loses even
more activity. The regenerator temperature declines steadily until the unit no longer
functions.
The operator should guard against getting behind in burning by:
1. Maintaining the normal regenerator temperature pattern.

2. Periodically checking that the color of the regenerated catalyst is not
increasing in greyness, indicating an accumulation of coke.
3. Anticipating changes in process conditions that increase coke production,
e.g., charge stock changes, decreases in combined feed temperature,
etc.
4. Carefully controlling the excess air level for 1-2 vol-% excess O2 in the
flue gas.
See the Emergency Procedures section of this manual for actions that should be taken
to correct this situation.
If the regenerator is operated with an excessive quantity of air, the regenerator

efficiency will decrease and cool the regenerator.
2.2.2.5 Dense Phase Temperature
The upper regenerator dense phase temperature is directly controlled by the heat
balance. The regenerator temperature is the heat balancing mechanism of the
regeneration process. Those changes in process conditions that tend to produce more
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coke also cause an increase in regenerator temperature. The increased
temperature reduces the catalyst/oil ratio that in turn reduces the coke production and
restores the balance.
The process changes that could cause an increase in the regenerator dense phase
temperature are:
1. An increase in charge specific gravity, average boiling point, or

Conradson Carbon level.
2. A decrease in charge characterization factor (UOP K).
3. Addition or an increase in bottoms recycle rate.
4. An increase in combined feed temperature.
5. An increase in reactor temperature.
6. An increase in reactor pressure.
2.2.2.6 Recirculation Catalyst Rate
A condition known as afterburning occurs when uncombusted CO does not begin to

burn to CO2 until the flue gases reach the upper regenerator. In this area, there is very
little catalyst to absorb the heat. This causes extremely high flue gas temperatures
that may seriously damage the cyclones or the flue gas line.
In the high efficiency regenerator, the carbon burn should take place in the combustion
riser to maximize the heat transfer to the regenerated catalyst in the upper regenerator
dense phase. If the combustor temperature is insufficient to burn all the carbon in the
combustion riser, burning will take place in the upper regenerator, decreasing the
regenerator efficiency. An indication of this type of afterburn is observed when the
upper regenerator dilute phase temperatures are greater than the dense phase
temperatures. This problem can be corrected by recirculating more hot catalyst from
the upper regenerator, which will increase the coke burning rate in the combustion
riser.
2.2.2.7 Regenerator Level
The upper section of the regenerator is the catalyst surge vessel of the unit. This level
will vary slightly with operating conditions but it is maintained by manually
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adjusting the rate of catalyst addition or withdrawal. Generally, fresh catalyst is made
up continually to maintain activity since the catalyst will deactivate at a certain
minimum rate, regardless of charge rate and composition. Usually there will be a
minimum daily catalyst makeup rate of 1-2% of the catalyst inventory. The makeup
rate necessary to maintain constant activity will tend to be less if the catalyst inventory
is small. This makeup normally results in an increasing catalyst level since this rate
should be greater than any loss rate. This requires periodic batchwise withdrawal of
equilibrium catalyst when the upper regenerator level gets high.
Operating with a low regenerator level should be avoided due to the decreased unit
stability that could arise. A low level will not provide the ability to absorb changes in
catalyst densities and circulation. A large regenerator catalyst inventory will absorb the
effects of minor upsets in operating conditions since the change in regenerator
temperature and catalyst circulation rate will be smaller.
2.2.2.8 Regenerator Pressure
An increase in the regenerator pressure will improve the catalyst regeneration, though
this variable is almost never used for that purpose. The effect of regenerator pressure
on slide valve differential pressures, main air blower power consumption, catalyst
entrainment, and cyclone efficiency is more important. Refer also to the reactor-
regenerator pressure balance discussion included in the Reactor section of the
Process Variables section.
Lowering the regenerator pressure will:
1. Increase the spent catalyst slide valve differential pressure.

2. Decrease the regenerated catalyst slide valve differential pressure.
3. Decrease the main air blower power consumption.
4. Slightly improve air distribution.
5. Increase catalyst entrainment to the cyclones.
2.2.2.9 Torch Oil
The torch oil nozzles permit oil to be sprayed into the combustor during startups as an
aid in heating up the catalyst inventory. Raw oil or circulating HCO is used, both of
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which have an IBP over 400°F (205°C), eliminating the danger of the torch oil
vaporizing before ignition when used during startup.
Torch oil should not be used during normal operations because its excessive heat can
sinter the catalyst resulting in deactivation. When it is necessary to use torch oil, care
should be taken to make sure the oil is properly atomized. A high concentration of the
oil in a small area can result in localized areas being hotter than the temperature
indicated by the regenerator’s temperature indicators. Never attempt to use torch oil
without catalyst recirculation and without a combustor catalyst density of at least 7
lb/ft3 (110 kg/m3).
2.2.3 CHARGE PROPERTIES
The Fluid Catalytic Cracking unit can accommodate wide variations in charge
composition and quality without seriously affecting the unit’s operation. However, any
change in the charge stock properties may require changes in process conditions to
maintain the unit at its optimum performance.
2.2.3.1 Boiling Range
The boiling point range of an FCC feed usually varies from an initial point of about
500°F (260°C) to an endpoint of about 1000°F (540°C). The distillation of
hydrocarbons in this high temperature range must be conducted under vacuum, and
corrected to atmospheric pressure, because thermal cracking of the sample will occur
above 700°F (370°C)
There are two boiling point ranges that are used to describe the lighter material in the
feed. These are percent over at 430°F (221°C), and percent over at 650°F (343°C).
The first value quantifies the amount of gasoline in the feed. This material may be
cracked, but only at a very slow rate. Most of it merely passes through the unit with
perhaps some small octane improvement. The octane improvement is somewhat
higher for cracked gasoline, as compared to straight run material. Because of this,
gasoline in the FCC feed is not desirable since it occupies space
which could be used to upgrade gas oil, and because it usually has a low octane
number. It would be better to remove this material in the feed pretreatment unit.
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The percent over at 650°F (343°C) is a measure of the light fuel oil in the charge. The
boiling point of 650°F (343°C) is chosen because it corresponds to the normal LCO
endpoint. This material will crack, but not to the same extent as the heavier material.
It will produce more coke than will the gasoline, but less than the heavier material.
The endpoint of an FCC chargestock may vary, depending to some extent on the
suitability of the material for cracking. The presence of heavy components that
contribute to coke formation is undesirable and is a good reason for not charging very
high boiling point material. These heavy components are referred to as coke
precursors and include polynuclear aromatics, organo-metallic compounds, and high
sulfur level compounds. The upper endpoint limit depends very much on the individual
feedstock and is determinable through operating experience.
2.2.3.2 Carbon Residue
The carbon residue of a stock, as determined by either the Conradson Carbon or

Ramsbottom methods, is an indirect measure of the coke producing characteristics of
a charge stock. An increase in the carbon residue of a charge stock will generally
result in an increase in regenerator temperature. However, this characteristic is not
always comparable for feeds from different crudes.
The carbon residue value can be a valuable indication of contamination in storage, or

of changes in the performance of the upstream units. Normally, an increase in carbon
residue will be accompanied by an increase in the metals content. A carbon residue
of 5.0 wt-% or greater is high for a suitable feedstock.
2.2.3.3 Characterization Factor – UOP K
The UOP K of a petroleum fraction gives an indication of its saturation and cyclization.
This value is a calculated rather than a measured quantity.
Refer to UOP Method 375 for an example of the UOP K calculation method. A high
UOP K value of 12.5 indicates a more paraffinic (saturated chain) hydrocarbon, while
a lower value of 11.2 occurs for a more aromatic (unsaturated cyclic) stock. Higher
UOP K paraffinic feeds crack easier yielding higher conversion at a given reactor
temperature
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2.2.3.4 Color
Color may be used as an indication of feed quality. Darker feeds tend to have higher
carbon residues, sulfur, and metal contents. Monitoring color is especially valuable
because operations personnel can easily make periodic rough visual color checks to
determine if the feedstock is satisfactory. The color of a desirable feed is typically near
4.5 as measured by ASTM Method D-1500, ASTM Color of Petroleum Products.
2.2.3.5 Gravity
A change in the gravity of the charge will be due to a change in either its boiling range
or in the type of crude from which it is derived. If the °API gravity increases because
of a more paraffinic crude, the following changes can be anticipated:
1. There will be a greater conversion at the same reactor temperature

since the charge will crack easier.
2. At a constant conversion, there will be a greater gasoline yield, with a

slightly lower octane.
3. The products will be less olefinic.
Note that the charge’s specific gravity relative to water at 60°F (15°C) is inversely
related to its °API gravity by the equation
2.2.3.6 Metals
Most crude oils contain metallic compounds which can enter the unit either by
entrainment or because the compounds are themselves volatile and are distilled with
the gas oils. Of the common metals, nickel, vanadium, sodium, iron and copper are
particularly harmful. They are permanently deposited on the catalyst during the
cracking reaction, and they change product distribution by promoting increased
hydrogen production.
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The results of metallic poisoning are:
1. An increase in the quantity of hydrogen in the off-gas stream. The most

valuable measure of the extent of metallic poisoning is the volume ratio of
hydrogen to methane (H2/CH4) in the product gas. A ratio of over 1.0 indicates
a significant degree of poisoning. A normal H2/CH4 ratio should be about 0.3-
0.8. In addition, a clean charge stock will produce about 50-100 SCF H2/bbl (9-
17 Nm3 H2/m3) at 60-70% conversion, whereas a heavily contaminated one
may produce 200 SCF/bbl (34 Nm3/m3) or more.
The increase in hydrogen production can result in an overloading of the Gas

Concentration unit wet gas compressor. Not only is there an increase in the
total volume of gas to be compressed, but the increase in the hydrogen content
lowers the gas density. This requires that the centrifugal compressor work
harder in order to achieve the same discharge pressure. This results in a
decrease in efficiency and an increase in utility costs. It may at times be
necessary to lower the compressor discharge pressure in order to handle the
increased volume of light gas.
2. An increase in olefin content of the LPG product. The propane (C3) fraction
normally contains about 70-75 vol-% olefins, but this can increase to as high
as 85 vol-% in an extreme case of poisoning. Sodium occasionally appears
in an an FCC charge because of inefficient desalter operation, or the injection
of caustic soda in a feed preparation unit. Sodium acts as a "flux" which lowers
the melting point of the catalyst and is probably the most common cause of
catalyst sintering and subsequent loss of surface area.
2.2.3.7 Nitrogen
Nitrogen acts as a temporary catalyst poison that reduces catalyst activity by blocking
the catalyst’s acid sites’ availability for promoting cracking reactions. A feed total
nitrogen concentration below 1,000 ppm is not detrimental to activity, but activity may
be affected at nitrogen levels above 1500 ppm.
Nitrogen in the feed is converted to ammonia (NH3) and cyanides (CN-) by the cracking
reactions, and nitrogen oxide compounds (NOx) and trace quantities of NH3 in the
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regenerator. The NH3 and CN- cause plugging and corrosion, while the NOx and NH3
in the flue gas may cause environmental problems.
2.2.3.8 Oxygen
Gas oils absorb oxygen in storage unless the storage tanks are gas blanketed. This
oxygen will combine with compounds in the raw oil at elevated temperatures of about
450°F (230°C) to form gums which foul heat exchange surfaces.
2.2.3.9 Sulfur
Sulfur is as undesirable in an FCC charge as it is in the feed to any refining unit since
it causes corrosion of equipment and also increases the difficulty and cost of treating
products. At 50% conversion, about 35% of the sulfur charged is converted to H2S. At
70% conversion, this figure increases to about 50%. The sulfur content of 400°F
(204°C) endpoint FCC gasoline will be somewhat over 10% of that of the raw oil charge,
but this increases rapidly as the endpoint is raised above 400°F (204°C). The higher
the sulfur content of the gasoline, the lower will be its lead response.
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2.3 PROCESS FLOW AND CONTROL
2.3.1 PROCESS FLOW
2.3.1.1 Reactor-Regenerator Section
A typical modern FCC with a high efficiency regenerator is shown in Figure 1. The
pumped raw oil charge is preheated by a series of cycle oil and main column bottoms
heat exchangers. The preheated raw oil and steam are introduced into the reactor
riser at a point approximately 20 feet (7 meters) up from the bottom of the riser. Here
the feed is contacted with a controlled amount of regenerated catalyst and lift media.
The catalyst flow is controlled to maintain a desired reactor temperature. The hot
regenerated catalyst vaporizes the feed and the resultant vapors carry the catalyst
upward through the riser with a minimum of back mixing. Cracking occurs as the
hydrocarbon vapors and catalyst travel up the riser. At the top of the riser the desired
cracking reactions have been completed and the catalyst is quickly separated from the
hydrocarbon vapors to minimize further cracking reactions.
The reactor product vapors flow through the reactor vapor line to the main column
where they are condensed and fractionated into gaseous co-products, FCC gasoline,
cycle oil products, and a heavy residual bottoms material.
During the cracking reaction, a carbonaceous by-product called coke is deposited on

the circulating catalyst. This catalyst (referred to as spent catalyst) drops from the
reactor chamber into the stripping section where a countercurrent flow of steam
removes both interstitial and some adsorbed hydrocarbon vapors. The stripped
catalyst flows from the reactor stripper through the spent catalyst standpipe to the
regenerator where the coke is continuously burned off. The catalyst flow through the
spent catalyst standpipe is controlled to balance the circulating catalyst flow by
maintaining a constant reactor catalyst level.
In the regenerator, the heat of combustion raises the catalyst temperature to the
1200°F-1375°F (648°C-746°C) range. The purpose of this regeneration is to reactivate
the spent catalyst so that when catalyst is returned to the reactor riser it is in the
optimum condition to perform its cracking function. The regenerator serves to burn the
coke from the catalyst particles and transfer heat to the circulating catalyst. The energy
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carried by the hot regenerated catalyst is used to vaporize and heat up the oil vapor
to the desired reaction temperature in the riser. It also provides the heat of reaction
necessary to crack the feedstock to the desired conversion level. Hot regenerated
catalyst is pre-accelerated with lift media (dry gas from the gas concentration unit
absorber section or steam) at the bottom of the reactor riser prior to contacting the
hydrocarbon feed stream further up the riser.
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Figure 1
UOP Fluid Catalytic Cracking Unit
with High Efficiency Regenerator
The regenerator is normally operated at conditions that achieve complete combustion

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of CO to CO2. However, the combustion temperature can be varied for partial CO

combustion if processing conditions allow a lower level of heat generation. The
regenerator is equipped with a catalyst recirculation standpipe that supplies hot
regenerated catalyst from the regenerator to the combustor to provide additional heat
to the combustor section. This will accelerate the combustion kinetics. The
recirculation catalyst flow is normally controlled to maintain the target combustor
temperature. The regenerator is also provided with an air heater that is used on startup
to supply heat to the system until the catalyst temperature is raised sufficiently for auto
regeneration. A catalyst cooler may be present to moderate the regenerator
temperatures when processing feeds with a higher level of con carbon. The catalyst
cooler generates HP steam.
Flue gas exits through cyclone separators to minimize catalyst entrainment prior to
discharge from the regenerator. The pressure of the exiting flue gasses is let down
either by passing through a turbine (power recovery unit) or else by passing through
the orifice chamber. The sensible heat of the hot flue gas is recovered in a flue gas
cooler steam generator. The catalyst lost from the regenerator is recovered in either
an electrostatic precipitator, a wet gas scrubber, or a third stage separator with an
underflow filter arrangement.
In order to maintain the activity of the working catalyst inventory at the desired level,
and to make up for any catalyst lost from the system, fresh catalyst is introduced into
the circulating catalyst system from a fresh catalyst storage hopper. An equilibrium
catalyst storage hopper is provided to hold regenerated catalyst withdrawn from the
circulating system as necessary to maintain the desired working activity and to provide
catalyst for startup.
2.3.1.2 Fractionation Section
Reactor product vapors flow to the main column where unstabilized gasoline and
gaseous, olefin rich co-products are sent overhead. The gasoline fraction is
condensed from the overhead material in the overhead condenser system and
collected in the main column overhead receiver. Some of the liquid from the overhead
receiver is returned to the main column as reflux. Net vapor and liquid are then routed
to the gas concentration unit.
Heavy naphtha and light cycle oil are recovered as sidecut products with the net yield
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of these materials being stripped for removal of light ends and sent to further
processing or storage. Net column bottoms exchanges heat with raw oil and cooling
water before flowing to storage. Heavy cycle oil or main column bottoms may be
recycled to the riser or to the feed surge drum. This is usually done during the low
conversion mode of operation when increased LCO production is desired.
Maximum usage is made of the heat carried to the main column by the hot reactor
effluent vapor. Circulating light and heavy cycle oils are utilized in the gas
concentration section for heat exchange purposes. Additional main column bottoms
streams are used for preheating raw oil feed and steam generation.
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Figure 2
FCC Main Column Flow and Control
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2.3.2 PROCESS CONTROL
2.3.2.1 Raw Oil Charge System
The Raw Oil Charge System provides feed to the unit, removes heat from the
fractionation section, and heats the charge to the desired reactor riser inlet
temperature.
Feed enters the charge drum (FA-21101) directly from one or more hot or cold feed
sources. The charge drum acts as a surge control to dampen process flow variations
from upstream units. Drum pressure floats on the main column pressure through a line
connected to the tower in the vapor space above the HCO draw tray. Drum level
control is maintained by a level controller that signals valves on the feed streams.
The raw oil is pumped on flow control through a series of heat exchangers, called the
feed preheat train, prior to entering the reactor riser through the feed nozzles. The raw
oil is heated by exchanging with the circulating LCO, net MCB, and circulating MCB.
Usually all streams except the circulating main column bottoms are flow controlled by
the operator. The final raw oil temperature is controlled by passing some oil around
the circulating main column bottoms exchanger. Figure 3 shows a typical feed preheat
train.
The feed preheat temperature is an important process variable. Lower feed preheat
temperature increases cat/oil and conversion, but requires more coke make to heat
balance the unit. If the feed preheat temperature is too low, increasing feed viscosity
can result in poor feed distributor atomization, with a resulting loss in unit selectivity.
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Figure 3
Feed Preheat System
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2.3.2.2 Optimix Feed Distributor Control
Elevated Optimix feed distributors are designed to maximize catalyst to oil contacting
by finely atomizing the heavy FCC feed and spraying those droplets uniformly over the
cross section of the riser. There are 3 stages of primary atomization of the oil through
the internals of the nozzle. After the oil has been sheared into discrete droplets, steam
is injected to assist in the final phase of atomization as the steam and oil exit the nozzle
tip.
Depending upon the characteristics of the feed being processed, steam may be
injected into the distributors in two locations. The primary atomization steam injection
is through a dedicated nozzle on the Optimix distributor. This steam mixes with the oil
as it sprays through the tip of the distributor into the riser. The secondary steam
injection is directly into the oil side of the distributor. This secondary steam will greatly
increase the atomization of the oil by increasing the pressure drop across the nozzles.
However, depending upon hydraulics in the feed system this is sometimes not
desirable if it limits the feed rate to the unit.
An operating map for the Optimix distributors is provided with the equipment
documentation. This map provides a guide for the recommended minimum and
maximum steam rates to the distributors as a function of feed rate. The minimum
steam rate is set at that which produces a tip exit velocity of 150 ft/s (45 m/s). This is
the suggested minimum velocity for acceptable coverage of the riser with the atomized
feed. The maximum recommended velocity to avoid tip erosion and catalyst attrition
is 300 ft/s (90 m/s). Within this steam range the steam use can be optimized, usually
by making changes and watching for a change in either the regenerator temperature
or the C2- yield. This total quantity of steam used includes any steam injected into the
oil side of the distributor. The operating map also includes a notation for the predicted
pressure drop across the distributor at various operating conditions. Optimization of
the feed steam is often done in conjunction with optimization of the lift zone velocity.
The optimum feed steam rate can change with changes in the feed viscosity, which
can result from significant changes to the feed composition or feed preheat
temperature.
It is very important to keep adequate steam purge to the distributors at any time there
is catalyst in the system without feed in the unit, such as startup and shutdown.
Inadequate steam purge can result in catalyst backfilling and plugging the distributor.
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Typical feed/oil piping is shown in Figure 4. An HIC valve is provided on each

individual feed and steam line to the individual distributors. These valves are used to
trim the flow to each distributor to balance the flows equally among the distributors.
Equal flow to each distributor is important to maximize the effectiveness of the
distributors.
Many emergency situations encountered on FCC units call for quick diversion of the
feed from the riser. Figure 4 shows the normal arrangement of the feed to riser bypass
system. When required, a control board mounted switch is activated which trips a
solenoid valve controlling the pneumatic signals to the feed bypass valves, causing
these valves to move to their failure positions, i.e. the valve in the line to the riser
closes and the valve in the bypass line to the main column opens. Normally, the next
course of action is to open the emergency steam to the riser wye to either maintain
catalyst circulation if the regenerated catalyst slide valve remains open or to clear the
riser of catalyst if the regenerated catalyst slide valve is closed.
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Figure 4
Optimix Feed Distributor
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2.3.2.3 FCC Catalyst Section – Reactor
The flow of catalyst between the reaction and regeneration sections is the heart of the
FCC process. This catalyst flow is quite large and can be in the range of 30 to 70 tons
of catalyst circulated each minute. Control of this flow (see Figure 1) is critical to good
unit operation. Hot regenerated catalyst exits the regenerator at a temperature around
1290-1355°F (700-735°C). This catalyst flows down through the regenerator
standpipe to the “wye” section of the riser where it contacts the lift gas and steam. This
catalyst flow is regulated by the regenerated catalyst slide valve. Reactor temperature
is controlled by the amount of catalyst required to raise the gas and oil streams to the
desired operating temperature. The reactor temperature controller controls the
opening of the regenerated slide valve through a low signal selector (LSS) to regulate
the amount of catalyst entering the reactor (see Figure 5). A safety feature
incorporated into all the catalyst slide valves is the pressure differential override. If the
pressure differential across the slide valve drops very low or becomes negative
indicating low or reverse flow, the pressure differential controller sends a signal to the
LSS to close the valve. This prevents oil from entering the regeneration section that
could result in very high temperatures and equipment damage.
Lean sponge gas from the gas concentration unit can be used as lift gas in the riser.
Lift gas flow is controlled at about 2 wt% of the fresh feed. The lift gas transports
regenerated catalyst up the riser to the feed injection point. Steam is also injected at
the bottom of the riser on flow control at approximately 2 wt% of the feed. Lift gas and
steam are controlled to maintain a minimum velocity of 10
ft/s (3 m/s) at operating conditions. A velocity of 15 ft/s (4.5 m/s) is the desired
rate. If not enough lift gas is available then more steam must be used to maintain at
least the minimum riser velocity.
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Figure 5
Regenerated Catalyst Slide Valve Control
The combined feed is mixed with atomizing steam at each of the feed distributors. This
mixture is then injected into the riser at a point about 20 feet (7 meters) above the lift
gas distributor where it meets the hot regenerated catalyst. The oil is immediately
vaporized with the resulting volumetric expansion forcing the catalyst/vapor mixture
up the riser to the reactor vessel. Cracking reactions take place in the 2-3 seconds
required for the catalyst and hydrocarbon vapors to reach the top of the riser. Catalyst
is quickly separated from hydrocarbon in the reactor VSS enclosure to reduce
overcracking. Cyclones further remove entrained catalyst particles from the
hydrocarbon vapors. The vapors exit the cyclones and flow to the main column for
separation. Recovered spent catalyst flows down the VSS enclosure and the cyclone
diplegs to the spent catalyst stripper section.
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Steam displaces any remaining hydrocarbon vapors from the catalyst in the reactor
stripper. Catalyst flows down over perforated baffle plates and steam flows upward
through the perforations in a counter current arrangement. The steam flow is controlled
at a rate of 1.5-3 lb (kg) per 1000 lb (kg) of catalyst circulation to achieve satisfactory
stripping.
From the stripper, spent catalyst flows out of the reactor into the spent catalyst
standpipe. Catalyst flow to the combustor is regulated by the spent catalyst slide valve
that maintains the reactor catalyst bed level. The level controller sends a signal
through the low signal selector to the valve actuator regulating the slide valve opening
as shown in Figure 6. Reactor catalyst bed level is controlled just above the bottom
of the VSS enclosure. This allows minimum catalyst inventory while fully utilizing the
stripping steam. Again, a pressure differential controller sends a signal to the LSS to
close the valve in case of low or negative pressure differential. This minimizes the
possibility of air entering the reactor during upsets.
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Figure 6
Spent Catalyst Slide Valve Control
2.3.2.4 FCC Catalyst Section – Regenerator
The high efficiency regenerator is divided into two sections. The lower section is called
the combustor where the spent, recirculation and cooled catalyst are mixed with air
and coke combustion occurs. The combustor operates in the fast fluidized regime of
fluidization. All the catalyst entering the combustor is transported up the combustor
riser into the regenerator where the regenerated catalyst disengages from the flue gas
and falls to the regenerator dense bed. The upper regenerator holds the cyclones,
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provides volume for the regenerated catalyst to disengage from the flue gas and
provides the surge capacity for catalyst in the system. There is no control
instrumentation on the regenerator catalyst level. A level recorder (LR) is provided to
monitor the regenerator catalyst level. The actual regenerator catalyst level changes
with catalyst additions, withdrawals and losses from the system.
An important feature of the high efficiency regenerator is the recirculation catalyst

standpipe and slide valve (Figure 7). The recirculation of hot regenerated catalyst from
the regenerator to the combustor is important in controlling the coke combustion rate.
By controlling the amount of catalyst recirculated, the following parameters are
controlled in the combustor: the precombustion mixing temperature, the catalyst
density, catalyst flux and catalyst residence time. This, in turn, allows the coke
combustion rate and catalyst regeneration to be optimized. The recirculation catalyst
slide valve is controlled through a low signal selector and a slide valve DPRC, similarly
to the other slide valves. The recirculation slide valve position is controlled by a TRC
located in the upper section of the combustor or by a density instrument (XIC) mounted
on the combustor vessel.
The regenerator pressure is indirectly controlled by operating the flue gas slide valves
from a controller that measures the differential pressure between the reactor and the
regenerator (Figure 7). Using PDRC control minimizes the effect of fractionation
section pressure surges on the catalyst circulation. The reactor- regenerator
differential pressure is generally chosen to roughly equalize the differential pressure
across the catalyst slide valves, though on occasion, considerations such as
minimizing the main air blower horsepower may govern.
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Figure 7
High Efficiency Regenerator Control System
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a. Air Blower and Flue Gas Control
Figure 8 shows a conventional control scheme for a turbine driven blower. Flow is
measured by the venturi in the discharge line. This FRC controls the speed of the
turbine that regulates air flow. A vent line, called a snort, is located on the air blower
discharge and is used to prevent air blower surge. The snort valve is controlled by the
anti-surge system.
The check valve in the air blower discharge line isolates the blower from the
regenerator if the blower trips, or if the regenerator over pressures. This closing action
is assisted by a spring loaded air cylinder, which operates when regenerator pressure
falls to a certain predetermined pressure differential with the air blower discharge. An
alternative arrangement sometimes used is to trip the solenoid valve of the air cylinder
on the check valve on a low flow signal from the air blower.
The typical flue gas system on an FCC is shown in Figure 9. This system is comprised
of double disc slide valves, an orifice chamber, a flue gas steam generator and an
electrostatic precipitator. Some installations use a wet gas scrubber in place of the
electrostatic precipitator.
The control scheme would remain the same in any case. A DPRC (differential pressure
recording controller) holds the proper pressure balance between the reactor and
regenerator by controlling the position of the double disc flue gas slide valves. There
is no differential pressure instrument across the flue gas slide valve because there is
nothing downstream that can cause over pressure and reverse flow.
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Figure 8
Air Blower (Turbine Driven)
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Figure 9
FCC Flue Gas System
Flue Gas Cooler Control
The flue gas cooler (SPE-21012) operates at low pressure. It takes flue gas at
essentially regenerator temperature and cools it to approximately 550°F (290°C) by
generating HP steam. Boiler feed water is brought in to the steam drum on level control
cascaded to an inlet flow controller. Before entering the steam drum the BFW is often
preheated through a combination of external steam preheat and an economizer
section at the outlet of the flue gas cooler. Often the external steam exchanger is
necessary to prevent the cool BFW from causing condensation on the OD of the
economizer tubes, which would result in corrosion from SOx acids. The economizer
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section of the cooler must also not cool the flue gas so much as to cause condensation
of these acid gasses in the downstream electrostatic precipitator (SPE-21013). Water
circulation through the tubes of the steam generation section is generally natural
circulation, with circulation ratios on the order of 15:1. The saturated steam from the
steam drum is sent to a steam superheater section at the flue gas inlet portion of the
flue gas cooler. In this section, the hottest flue gas is used to superheat not only the
steam from the flue gas cooler, but also the steam from any main column bottoms
steam generators (EA-21108A/B/C) and catalyst coolers. Because the degree of
superheat cannot be controlled, a small stream of boiler feed water is injected into the
superheated steam on temperature control to control the degree of superheat.
Continuous blowdown is taken from the steam drum at a rate of approximately 5% of
the incoming BFW. In order to prevent carryover of large amounts of water to the HP
steam header, the inlet BFW valve fails closed. The relatively small desuperheater
valve that directs the BFW to the superheater outlet fails open to prevent overheating
the HP steam header. The tubes of the flue gas cooler are not designed to run dry.
Thus, if BFW flow to the flue gas cooler is lost and cannot be restarted within a few
minutes, the FCC flue gas flow must be stopped. Most often this requires that the FCC
be shut down.
Torch Oil Nozzle Control
Figure 10 shows a typical torch oil arrangement for an FCC regenerator. The torch oil
nozzles provide a means of injecting heavy oil, such as raw oil feed, into the
regenerator when extra heat is needed, e.g. during startup. Details of the nozzle will
be described in the section covering equipment. Control of the torch oil flow and the
torch oil atomization steam is often by hand control on older units. New unit designs
usually use a board mounted flow controller (FRC) with a split range output to the torch
oil flow and the torch oil atomization steam. The torch oil assembly is provided with a
continuous steam purge to the annular space around the torch oil nozzle to keep it
clear of catalyst. This purge steam flow is regulated to less than 50 lb/hr (25 kg/hr)
steam with a restriction orifice. In addition, a small flow of steam is often sent through
the nozzle when not is not being fired (no oil flow) to help cool the nozzle and keep
the nozzle from plugging with catalyst when not in use. This cooling steam flow is also
regulated with a restriction orifice.
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Figure 10
Torch Oil Instrumentation
2.3.2.5 Direct Fired Air Heater (DFAH) (BA-21001)
Figure 11 shows a direct fired air heater, present on all FCC units between the blower
and the combustion air inlet to the regenerator. The air heater is used for refractory
curing and dry out following repair or renewal of regenerator linings, as well as during
normal startup to heat the regenerator catalyst inventory. The DFAH outlet
temperature is controlled by the fuel gas rate. Because air heater misoperation can
cause damage to regenerator internals, a high temperature shutdown is provided. For
additional safety, the air heater will also shut down on low air flow and loss of flame
detection from a flame sensor.
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Figure 11
Direct Fired Air Heater
2.3.2.6 Fractionation Section
2.3.2.6.1 Main Column Control
The main column (DF-21101) is the first step in the product separation sequence. The
superheated reactor vapors need to be cooled so that fractionation can be conducted
and scrubbed of entrained catalyst. In large measure, operation of the main column
becomes an exercise in controlled heat removal coupled with sufficient liquid-vapor
contacting to effect the desired degree of fractionation into desired product streams,
namely main column bottoms (CLO), heavy cycle oil (HCO), light cycle oil (LCO),
heavy naphtha (HCN), unstabilized gasoline and wet gas. CLO, HCO, LCO and HCN
are taken as products directly from the main column, although on many FCC units
HCO and HCN are not removed from the unit as discreet product streams. Main
column sidecut products are often steam stripped in sidecut strippers for flash point
adjustment. The unstabilized gasoline and wet gas are subjected to further separation
in the gas concentration section. The arrangement and integration of heat exchange
from an FCC main column varies from refinery to refinery based on the specific
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requirements and economics of a given installation. The following discussion

describes typical heat exchange circuits used on an FCC unit. Figure 2 shows an
simplified FCC main column schematic.
2.3.2.6.2 Main Column Bottoms Pumparound Circuit
The main column bottoms system is designed to desuperheat the reactor vapors,
condense the bottoms product and scrub entrained catalyst particles from the reactor
product gases. Main column bottoms (MCB) is removed from the bottom of the main
column and sent to a circulating bottoms/raw oil exchanger (EA-21101A/B, EA-
21102A/B, EA-21104A/B) and one or more steam generators(EA-21108A/B/C). MCB
is also sometimes used to provide heat to reboilers. The incoming reactor vapors are
desuperheated by circulating a large stream of cooled slurry oil over the disk and donut
trays where it acts to desuperheat the reactor vapors as well as flush catalyst fines out
of the column as shown in Figure
12. The cooled bottoms circulation rate is normally set at 120% to 150% of the feed
rate or 14.7 m3/hr per square meter (6 gpm/ft2) of column cross sectional area,
whichever is greater. The bottoms temperature is maintained at 670-690°F (354-
366°C) to minimize coking in the slurry circuit. The bottoms material in the column is
operating at its bubble point, so bottoms temperature is controlled by controlling the
composition of the bottoms material. To control the bottoms composition, the LCO
draw rate is varied. If the bottoms temperature is too high, the operator should
decrease the LCO draw rate. This will allow more light material to slump down the
column and thus decrease the bottoms temperature. Coking rate is a function of time
and temperature, thus the LCO draw rate must be varied to maintain the bottoms
temperature below the coking temperature. A cooled stream of circulating main
column bottoms, taken from the outlet of the steam generators can be returned as
quench to the main column bottom to subcool the bottoms material and lower the
temperature when necessary. Care must be taken not to starve the slurry circulation
to the top of the disk and donut section when diverting bottoms pumparound to quench.
The minimum spillback is provided for minimum slurry circulation during turndown
operation. This ensures enough oil is returned to the main column adequately covering
the disc and donut trays, thereby cleansing the reactor vapors of catalyst fines and
preventing coke formation on the disk and donut trays due to insufficient liquid flow
over the trays.
During normal operations the heat input from the circulating main column bottoms to
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reboilers and preheat exchangers will be set by product and process considerations.
Heat input to the steam generators is the only variable available to the operator for
adjustment. Bottoms flow to the steam generators can be adjusted to change the
amount of heat rising up the column thus increasing or decreasing the column top
reflux rate which acts to heat balance the column.
Each exchanger in the main column bottoms pumparound circuit is designed for oil
containing catalyst particles. Main column bottoms flows through the exchanger on the
tube side and the velocity must be kept between 3.75 ft/s and 7.0 ft/s (1.14 m/s and
2.13 m/s). If the oil velocity falls below the minimum, catalyst will begin to accumulate
on the tube walls and slowly plug the tube while greatly reducing heat transfer. If the
velocity is above 7 ft/s (2.13 m/s), the tube walls may experience erosion leading to
premature failure. The rates required to meet these velocities must be calculated for
each exchanger before startup.
Figure 12
Main Column Bottoms Circulation and Product
Bottoms product is withdrawn to maintain a steady bottoms level in the main column.
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The product stream is cooled by heat exchange with a charge preheat exchanger and
a water cooler. Bottoms product flows through the tubes in the feed preheat exchanger
with the above mentioned velocity constraints. Removal of catalyst fines from the
bottoms product is an option which may be included depending on the end use of the
bottoms product.
2.3.2.6.3 HCO Pumparound Circuit
HCO is withdrawn from the column and normally used to provide heat to the charge
preheat exchanger and the debutanizer reboiler (EA-21213).. Occasionally, HCO is
also used to generate steam and reboil side cut strippers such as a heavy naphtha
stripper (see Figure 13). HCO flow to each of these exchangers is regulated by a flow
controller. Each controller is set by the operator to achieve desired product or process
specifications. If a steam generator is used, then the HCO pumparound heat removal
can be varied to some extent independent of process or product requirements.
The HCO circulation rates also provide proper reflux in the HCO section of the column.
A decrease in heat removal from the HCO circuit will require an increase in heat
removal elsewhere in the column. For example, if less heat is required by the
debutanizer reboiler, HCO circulation will be decreased. Lower circulation reduces
reflux to the HCO section of the main column, increasing the amount of vapor rising
up the column. If the excess heat is not removed in another pumparound circuit, the
reflux to the top of the main column will increase to remove this heat.
HCO product (if any) can be removed through a stripper for flash point adjustment.
The amount of HCO product produced will depend on reactor operating conditions,
feed quality and catalyst type. The plant operator will make adjustments in HCO, LCO
and naphtha draw off rates to maintain target boiling ranges for these products. If HCO
is taken as a product it would first be cooled against raw oil in a charge preheat
exchanger and then sent through a water cooled product cooler on flow control.
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Figure 13
Heavy Cycle Oil Circulation
The HCO circuit also provides torch oil to the regeneration section for start-up and
emergencies and flush oil to the main column bottoms pumps. A spillback to the main
column is provided for control of internal reflux. The spillback operates off a level
controller on the HCO drawoff tray.
2.3.2.6.4 LCO Pumparound and Product Circuit
Circulating LCO normally provides heat to the gas concentration unit stripper reboiler
(EA-21210) and the debutanizer feed exchanger (EA-21212) as shown in Figure 14.
Flow to each exchanger is regulated by a flow controller that is set according to
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process requirements. A stream of LCO, after heat exchange at the stripper reboiler,
is sent to the sponge absorber (DA-21202) as “lean” oil to adsorb light gasoline range
components from the light gas in the gas concentration section. The “rich” oil from the
sponge absorber is returned to the main column with the cooled LCO circulation
stream, providing internal reflux for the main column LCO section.
Most units contain an LCO stripper (DS-21102) for LCO product flash point adjustment.
Depending upon the plant arrangement, light ends in the LCO can be removed either
by steam stripping or by reboiling the liquid using heat from the circulating HCO. The
LCO product may exchange heat with the raw oil feed stream before being cooled with
water in a product cooler (EA-21103A/B) and being sent to storage. Flow to storage is
set by a flow controller. The LCO draw rate also controls the main column bottoms
temperature. The amount of LCO produced depends upon operating conditions, feed
quality and catalyst type. Stripped LCO is available for use as torch oil, instrument
flush and pump gland seal oil.
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Figure 14
Light Oil Circulation and Product
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2.3.2.6.5 Naphtha Pumparound and Product Circuit
Naphtha product is typically withdrawn through a side cut stripper column in order to
remove light ends for vapor pressure adjustment. The naphtha stripper bottoms
product is cooled with water in a product cooler and then sent to storage or treating on
flow control (FRC). The portion of the naphtha draw from the main column which is not
stripped as product is pumped and used for heat exchange with raw oil feed, water or
other low temperature streams such as a C3/C4 splitter reboiler (EA-21402) and
returned to the main column as internal reflux for the main column naphtha section.
Figure 15 shows a flow scheme for the naphtha pumparound circuit.
2.3.2.6.6 Main Column Overhead System
Reactor product vapors contain large quantities of light gas and gasoline vapors that
pass through the entire main column as saturated gases. These products are
condensed in the overhead condenser (EC-21102), the trim condenser (EA-
21107A/B/C/D), and separated in the main column overhead receiver (FA-21102). A
quantity of the condensed hydrocarbon liquid (unstabilized gasoline) is pumped to the
main column as reflux (see Figure 16).
Reflux to the main column controls the overhead vapor temperature. This temperature
determines the endpoint of the gasoline product. The reflux also heat balances the
column. If heat removal from one section is changed the reflux rate will respond in the
opposite direction to maintain a constant top temperature. For example, if more heat
is required in the feed to the debutanizer, LCO circulation will be increased to provide
the heat. The increase in LCO circulation will condense more vapor rising up the
column. Less heat will reach the top of the column. The top temperature controller will
then reduce the reflux flow to maintain the column top temperature, thus heat
balancing the column.
The unstabilized gasoline liquid in the receiver not used as reflux is pumped to the gas
concentration unit on receiver level control. Gas flows to the suction drum (FA-21201)
of the wet gas compressor in the gas concentration unit. Water from the overhead
receiver is pumped to the waste water treating unit.
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Figure 15
Heavy Naphtha Circulation Product
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Figure 16
Main Column Overhead System
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2.4 TROUBLESHOOTING
2.4.2 FCC MAIN COLUMN BOTTOMS SYSTEM FOULING
The most common form of fouling in the FCC Slurry System is coking. There are three
primary variables that influence bottoms coking. These are temperature, residence
time, and slurry quality.
1) Experience has shown that the rate of coke build-up increases greatly when
the bottoms temperature is allowed to rise above 700°F (370°C). Most
operations try to maintain the bottoms temperature below 690°F (365°C) to be
on the safe side. When fouling is observed, it is often prudent to lower the
temperature below 680°F (360°C).
2) Residence time also has a significant impact on coke build-up. Residence time
in this context refers only to the time that the slurry spends in the column and
not in the entire system. Once the slurry is removed from the column and
passes through the heat exchange system, the temperature is lowered and the
propensity for coking is stopped. For convenience, UOP prefers to express
residence time in terms of slurry circulation. Typically, the minimum circulation
rate required to prevent coking is 6 gpm/ft2 (14.67 m3/hr per m2) of column
cross-sectional area but not less than 150% of the design feed rate. Most
FCCU's have no problem in meeting this minimum circulation criteria. The
circulation required to heat balance the main column is usually above this
minimum. If more circulation is required, a hot oil bypass which bypasses the
exchangers and returns oil directly to the main column has been installed.
3) The quality of the slurry has a large effect on its coke making tendencies. Unlike
temperature and residence time, it is more difficult to control slurry quality. The
major variables that effect slurry quality are: feedstock type, catalyst type,
reactor severity, and main column operation.
a) Heavy feeds and very paraffinic feeds tend to produce slurries that are
more susceptible to coking. The tendencies of these feedstocks to coke
can often be judged by monitoring changes in contaminants such as
Conradson Carbon and nitrogen.
b) Lower matrix activity catalysts tend to produce slurries that are reactive
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and more susceptible to coking.
c) Low reactor severity operations tend to produce slurries which are not fully
reacted and which may crack and form coke in the main column.
The coke formed through mechanisms (a-c) can often be significantly

reduced or eliminated by minimizing the coke precursors leaving the
reactor system. This can be achieved by increasing reactor severity
through a combination of reactor temperature and catalyst activity. The
increase in severity aids in the destruction of coke precursors.
Reformulation of the catalyst with additional bottoms cracking ability
(normally a higher matrix activity) to make a more stable aromatics bottom
product is also a key to correcting fouling problems. It should be noted that
the above changes may increase the regenerator or increase the unit coke
make and require more regeneration air. The reduction of fouling in this
case becomes an economic tradeoff.
Coke formation in the bottoms system can also be addressed operationally

through mechanisms d) and e).
d) When running heavy feeds with a low matrix activity catalyst at low
conversion, it is still possible to minimize coking with control changes of
the main column. As an initial guideline, UOP recommends that the light
cycle oil draw rate be controlled to limit the slurry gravity at a minimum of
2°API or the slurry viscosity at a maximum of 25 Cs at 99°C. With time
these limits can be either increased or decreased to minimize coking in the
main column bottoms circuit.
e) Often times, the cause for coking in the bottoms system is found to be raw
oil leaking into the bottoms system from the feed bypass valve or the feed
system pressure relief valves. These systems should be carefully
inspected for leaks.
Refiners who wish to produce slurry for the carbon black market may need to push the
slurry API very low via reactor severity and main column operation. To avoid main
column bottoms coking for this scenario, it may be necessary to quench (subcool) the
slurry in the bottom of the tower with cooled slurry exiting one of the steam generators.
Piping and instrumentation is provided for this operation.
Usually slurry catalyst content does not directly cause coking problems. Plugging
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problems can occur when large quantities of catalyst are lost from the reactor due to
mechanical problems, operational upsets, and catalyst structural problems, or when
slurry heat exchanger velocities are low. To prevent catalyst plugging or erosion in the
exchangers, UOP recommends maintaining a maximum velocity of 7.0 ft/s (2.13 m/s)
and a minimum velocity of 3.7 ft/s (1.14 m/s) in the slurry exchanger tubes.
In general, the optimum velocity is 5.7 ft/s (1.75 m/s). Straight tube construction is
recommended. It is important to think of these numbers when changing raw oil charge
or exchanger flow rates.
Another form of fouling is the polymer type of deposit, typically in the cool end of the
net slurry rundown circuit. There is some evidence to suggest that it is similar to coking
and can be addressed in the same fashion as items (a-c) above, by increasing reactor
severity through a combination of reactor temperature, catalyst activity, and bottoms
cracking matrix. Another way to address this problem is to increase the coolest
temperature the slurry is exposed to.
Some refiners have had success retarding polymer formation with inhibitors. These
inhibitors tend to be expensive and injection must be initiated with a clean exchanger.
These materials may prevent polymer buildup, but experience has shown that they do
not do a good job of removing buildup once it has formed.
2.4.3 CATALYST LOSS

The four primary indicators of catalyst loss are:
1. Increased MCB BS&W content

2. Increased Regenerator Flue Gas fines content
3. Increased catalyst make-up rates at the same withdrawal rate
4. Decreased catalyst withdrawal rates at the same catalyst make-up rates
Changes in catalyst loss rates can result from:
1. Increased superficial velocities in the reactor or regenerator resulting in

increased loadings to the cyclones
2. Misoperation
3. Mechanical damage
4. Improper manufacture of the catalyst, i.e., increased softness or increased
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fines content
5. Physical damage to the catalyst
6. Improper functioning of the cyclones
7. Faulty instrumentation readings
1. Superficial velocities above 3.8 ft/s (1.16 m/s) in the regenerator will generally
increase the entrainment of catalyst into the freeboard space above the catalyst
bed. During unit startup it is not unusual for the regenerator to be at a low
pressure resulting in high superficial velocities.
2. If the equipment (e.g. air grid, feed distributor, stripping steam ring) is operated
substantially above their design values, then the high velocity can cause
catalyst attrition.
3. Mechanical damage can result in increased attrition of the catalyst and

therefore higher catalyst losses since the cyclones generally only retain
material larger than 20µm. Common examples of mechanical damage are
regenerator air grid cracks or holes and feed distributor cracks. If there are
cracks in the plenum head or holes in the cyclones, then catalyst bypassing will
occur and a larger average Particle Size Distribution (PSD) will be observed.
4. Certain catalysts will have higher attrition rates or have higher fines in the fresh
catalyst than others. Fresh catalyst with high fines content usually shows up as
regenerator losses. Catalyst with a high attrition index will show up as both
losses from the reactor and regenerator.
5. Catalyst particle strength can be detrimentally affected by thermal or chemical

damage. Thermal damage is usually caused by plant upsets or extended use
of torch oil. Catalyst poisons affecting the strength of catalyst include Ca and
K.
6. Improper function of cyclones can be caused by low inlet velocities resulting in

low efficiencies, plugged diplegs or mechanical damage resulting in a pressure
imbalance.
When troubleshooting continuous elevated catalyst losses, it is very important to have

a good baseline of “normal” losses, including the total tons/day lost and the typical
particle size distribution of the losses. When experiencing high catalyst losses, the
atypical data can be compared to the typical data to narrow the focus of the
troubleshooting. For example, if the particle size distribution of the losses is much
smaller than normal, catalyst attrition is the likely cause.
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It is recommended that the refiner collect the following baseline data:
a. Weight flow of catalyst in the net slurry. This can be determined by multiplying
the net slurry mass flowrate by the wt % ash content of the net slurry.
b. Weight flow of catalyst collected by the flue gas emissions control equipment -
ESP, TSS or flue gas scrubber. Note that the emissions control equipment will
not collect 100 % of the catalyst leaving the regenerator. Some will escape to
the stack.
c. Weigh flow of catalyst escaping the stack. This must be collected isokinetically
by a special testing company qualified to do this work.
d. Weight flow of fresh catalyst and additives entering the unit.
e. Weight flow of equilibrium catalyst withdrawn from the unit.
f. Particle size distribution of the ash in the net slurry, catalyst collected by the
emission control equipment, stack isokinetic sample, fresh catalyst and
additives and equilibrium catalyst. All size distributions should be determined
using the same instrument from the same laboratory.
It is recommended that a complete round of baseline testing including the stack

isokinetic test along with particle size distribution for each location be conducted at
least once per year.
A catalyst mass balance including the net slurry ash, emission control equipment
collection, fresh catalyst and additive addition and e-cat withdrawal should be
conducted weekly.
The e-cat PSD should be monitored and trended with each update of the e-cat data
sheet from the catalyst supplier. Likewise, the fresh catalyst and additive PSD should
be monitored and trended with each new certification sheet from the catalyst supplier.
The net slurry ash PSD should be monitored and trended at least monthly. The catalyst
supplier will usually do the net slurry ash PSD if requested. Ask your catalyst supplier
to provide detail analysis between 1 and 20 microns for all the samples. They will have
this information, but will not provide it on the e-cat data sheets unless specifically
requested
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2.5 SPECIAL PROCEDURES
2.5.2 CATALYST SAMPLING

NOTE: When collecting hot catalyst samples, gloves and long sleeved Nomex
coveralls should be worn. Use a metal container to collect the catalyst sample.
The following procedure is recommended for collecting catalyst samples. Refer to

Figure 1.
Regenerated Catalyst Sample
1. The slide valve differential pressure controller should be switched to manual

since purging the sample connection could upset the slide valve differential
pressure controller.
2. Check that all blast and sample connection valves are closed, then open
sample valve E and steam valve B. Vent steam to the atmosphere until it is hot
and dry.
3. Close sample valve E and open nozzle valves F & G. Steam purge the sample
line into the standpipe.
4. Open sample valve E and reduce the steam flow through valve B until a small
flow of catalyst is obtained. If catalyst does not flow out of sample valve E, blast
the standpipe through steam valve C.
5. Take the sample and then close sample valve E.
6. Open steam valve B and purge into the standpipe.
7. Close nozzle valves F & G, and then steam valve B.
8. Open sample valve E
9. Put the slide valve differential pressure controller back in automatic control.
Spent Catalyst Sample

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Spent catalyst analysis is not required for routine process monitoring. Collecting a
spent catalyst sample requires special equipment and procedures to preserve the
composition of the coke on the catalyst once removed from the process. Contact UOP
before attempting to collect a spent catalyst sample.
2.5.3 BLASTING CATALYST STANDPIPES

NOTE: Air should not be used when purging into the reactor or associated
standpipes.
Blast and sample connections are located just above each slide valve. Blast only
connections are located at various other locations in the standpipes. These
connections are used to clear the standpipes of any plugs that might occur.
The following procedure is recommended for blasting at blast and sample connections.
A similar procedure can be used for blasting at blast only connections. Refer to Figure
1.
1. Place the appropriate slide valve controller in manual when blasting a

standpipe.
2. Check that all blast and sample connection valves are closed, then open
sample valve E and steam valve C. Vent steam to the atmosphere until it is hot
and dry.
3. Close sample valve E and open nozzle valves F & G. Purge steam into the
standpipe until the plug is cleared.
4. Close nozzle valves F & G and steam valve C.
5. Open sample valve E.

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Figure 1
BLAST AND SAMPLE CONNECTIONS
2.5.4 DIRECT FIRED AIR HEATER
The direct fired air heater is used to heat up the circulating catalyst inventory during
startup. The heater is also used to dry out refractory in the regenerator and reactor
during commissioning and following major refractory repairs. The heater can also be
used continuously during normal operations when required to maintain sufficient
regenerator temperature required for combustion kinetics.
NOTE: The direct fired air heater is designed for continuous firing without
continuous outside operator monitoring. However it is recommended that the
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air heater be continuously monitored during startups until feed has started and
the unit is stable. Refer to the Normal Startup procedures for monitoring details.
NOTE: Unlike conventional fired heaters, the direct fired air heater operates at
process pressure. The fuel gas instrumentation (including the Emergency
Interlock System) is designed to monitor and control the differential pressure
between the fuel gas supply pressure and the process pressure.
The heater can only be fired when the main air blower is running. A local temperature
indicator is provided for the outlet of the air heater so the outside operator can monitor
the temperature when the heater is first fired up.
The Emergency Interlock System will shut off the fuel gas supply to the heater if any
of the following occur:
• Flame failure as monitored by flame detectors

• High heater outlet temperature
• Low fuel gas or pilot gas differential pressure
• Loss of main air
• Loss of water level in the heat recovery steam generator.
The heater is equipped with two removable plume type pilot/igniter assemblies. Each
assembly is equipped with fuel gas and combustion air connections. Either one may
be used during operations, with the other held in standby.
Refer to the manufacturer’s operating manual for detailed operating information. The
general heater startup steps are:
1. The main air blower must running and the heat recovery steam generator must
be inventoried with boiler feedwater before the heater can be started.
2. Adjust the damper to the minimum position (minimum air to the burner block)
to prevent blowing out the pilot flame with main air.
3. Close the block valves adjacent to both pilots and the main burner. Open the
combustion air to one of the pilots, and purge to remove any moisture. Place
the main burner pressure differential controller in manual with a set point of 0%
open. Pull the blind in the air heater’s fuel gas line.
4. Reset the pilot gas solenoid valves.

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5. Press the button on the local control panel supplying power to the selected pilot
igniter. Then unblock the ¾” fuel gas line supplying gas to the selected pilot
burner.
6. Once the pilot is ignited, open the 1” fuel gas line to the pilot. This will provide
a strong plume pilot resistant to flameout.
7. When the plume pilot has been lit, reset the fuel gas solenoid valves. Open the
main burner block valve and slowly open the pressure differential control valve
until a flame is obtained. Place the heater in automatic temperature control
when operations are stable.
NOTE: The ignitors can be retracted while leaving the plume pilots in place.
After the main burner is lit, the igniters should be retracted to prevent damage
to the tips.
8. While the air heater is relatively simple to operate, the following precautions
should be observed:
a. The fuel gas to the heater must be free of any liquid. Slugs of hydrocarbon
liquid can cause major damage as unatomized liquid fuel causes
temperatures to rise very rapidly.
b. The heater is designed so the flame length does not exceed the mid point
of the main heater chamber to prevent damage to the air distributor inside
the regenerator. The flame should not be visible from the sight port at the
outlet end of the heater. If the flame is visible, firing must be reduced.
9. Any time the heater is shut down, allow 10 minutes before resetting the pilot
gas and fuel gas solenoid valves so that any combustibles will be purged out
of the heater.
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2.5.5 FLUSHING SYSTEM

The main column bottoms contains catalyst which can settle out and plug level
instruments, relief valves and small piping, and which can erode pumps and block
valves. The flushing oil system flushes this equipment with clear oil to prevent plugging
and erosion. The flushing oil system is also used to flush slurry oil out of spare pumps
and exchangers to ensure the slurry does not set up in the equipment and piping when
not in service.
The throat bushing and wearing rings of the main column bottoms pumps are flushed
with hot heavy cycle oil (HCO) taken from the circulating HCO pump discharge. Hot
material is used to avoid the stresses that would result if cooled oil was injected into
the hot pump cases. Heavy cycle oil is used since lighter material could vaporize and
cause the pump to cavitate. The main column bottoms pump bellow seals are also
flushed with HCO. A cooler is provided with the seal reservoir to keep the sealing liquid
below 350°F (175°C). Raw oil is used in place of HCO for pump flushing during startup.
Light cycle oil (LCO) is used for flushing level instruments, relief valves, block valves
and spare equipment and piping. This flushing oil is taken from the LCO product cooler
outlet. The flow of flushing oil to level instruments and relief valves is controlled by a
restriction orifice at each point of service. Raw oil is also used in place of LCO for
flushing during startup.
2.5.6 REACTOR VAPOR LINE BLIND

The reactor vapor line blind is located just upstream of the main column. Installing or
removing this blind is one of the more hazardous operations in a refinery because the
operators can be exposed to high temperatures and H2S. Operators involved in these
operations must wear positive pressure fresh air masks and fire resistant clothing.
Removal
For a normal startup, UOP recommends a “blind out” procedure. In this procedure, the
blind is removed before any hydrocarbon is added to the main column. In this situation,
the blind can be removed at any time prior to introducing hydrocarbon into the main
column.
In certain situations, a “blind in” startup is preferred. This means that at least some
hydrocarbon has been added to the main column before the blind is removed.
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Refer to Figure 2. The following steps should be followed:
1. Close the spent and regenerated catalyst slide vales.
2. Fully open the reactor vent valve located upstream of the blind. Steam out the
reactor in accordance with the Normal Startup procedures.
3. Shut down the main air blower. Even though the slide valves are closed, they
are not designed to be leak tight. Shutting down the blower will prevent air from
entering the main column.
4. Stop all fuel gas to the main column.
5. Blanket the lower part of the main column with steam from the LCO side
stripper and from the steamout connections at the bottom of the main column.
6. Throttle back the steam supply to the reactor and main column to achieve a
maximum pressure of 1” wg (25 mm wg) on both sides of the blind before
attempting to remove.
7. Purge both sides of the vapor line with steam from the steam connections just
upstream and downstream of the blind. Open the two drains upstream and
downstream of the blind to allow condensate to drain.
8. Remove the reactor vapor line blind and insert spacer.
9. Close the reactor vent valve and install the adjacent blind.
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Figure 2
MAIN COLUMN BLIND
Installation
The blind installation procedure is similar to the removal procedure. The following
steps should be followed:
1. Close the spent and regenerated catalyst slide vales.
2. Steam out the reactor in accordance with the Normal Shutdown procedures.
3. Shut down the main air blower. Even though the slide valves are closed, they
are not designed to be leak tight. Shutting down the blower will prevent air from
entering the main column.
4. Stop all fuel gas to the main column.

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5. Blanket the lower part of the main column with steam from the LCO side
stripper and from the steamout connections at the bottom of the main column.
Continue to steam out for 30 minutes after fuel gas is stopped.
6. Remove the blind in the reactor vent line and completely open the reactor vent
valve.
7. Throttle back the steam supply to the reactor and main column to achieve a
maximum pressure of 1” wg (25 mm wg) on both sides of the blind before
attempting to remove.
8. Purge both sides of the vapor line with steam from the steam connections just
upstream and downstream of the blind. Open the two drains upstream and
downstream of the blind to allow condensate to drain.
9. Install Reactor Vapor Line Blind.
2.5.7 OPTIMIX FEED DISTRIBUTOR BALANCING

The Optimix feed distributors should be balanced using the following procedure. Refer
to the documentation provided with the equipment for an operating chart of the feed
distributors:
1. Set the raw oil feed rate near the design rate.
2. Set the primary atomizing steam at the design rate. Set the secondary
atomizing steam at the design rate, or shut off if the design rate is zero.
3. Open wide all the HIC valves in the raw oil lines to each distributor.
4. Record the flowrate to each distributor. The flowrate to each distributor should
be within 5% of the average. If one of the feed distributors exhibits substantially
higher or lower flowrate than the average, this may indicate distributor damage
or plugging.
5. Adjust the HIC valves so the flow to each distributor is within 2% of the average.
Record the flowrate and pressure drop across each distributor.
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2.5.8 CATALYST ADDITION SYSTEM

Fresh catalyst and additives should be added to the unit at a uniform pace continuously
throughout the day. This provides a uniform catalyst activity and allows operation at
optimal profitability.
A weigh scale based catalyst addition system is provided for this purpose. Refer to
Figure 3. The injection system controls total flow by weighing each batch of catalyst
before it is injected into the regenerator. The controller operates 3 on-off valves (inlet,
outlet and pressure) to load, pressure and inject the catalyst into the addition line. The
operator sets both the desired overall mass flow rate and the batch weight via the
distributed control system. These setpoints are then transmitted to the controller.
Once the system is activated, the controller will open the inlet valve, load the desired
amount into the load hopper, and then close. The system then pressures up the load
hopper and opens the outlet valve to inject the catalyst. The time interval between
batches is determined by the control computer and adjusted in order to achieve the
desired daily flow rate.
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Figure 3
WEIGHT BASED CATALYST AND
ADDITIVE ADDITION SYSTEM
2.5.9 CONTINUOUS CATALYST WITHDRAWAL SYSTEM

Equilibrium catalyst should be removed from the unit at regular intervals. This provides
a uniform catalyst level in the regenerator. This also provides a constant catalyst
inventory which allows finer control of the catalyst activity and additive concentration.
A continuous catalyst withdrawal system is provided for this purpose. Refer to Figure
4. The operator sets the number of cycles per day and the duration of the cycle.
To operate the system, perform the following steps:

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1. Line up the catalyst withdrawal lines to the equilibrium catalyst hopper and open
the vent line at the top of the hopper.
2. Open both block valves at the wall of the regenerator and depress the start
switch. The logic system will begin by opening the carrying air to the withdrawal
line. After five minutes, the catalyst withdrawal valve will open and remain open
for the duration of the cycle, and then close. The carrying air will remain on for
an additional five minutes to clear the catalyst withdrawal line. The system will
then remain idle until the next cycle commences.
3. The carrying air flowrate is engineered to minimize temperature induced

stresses in the catalyst withdrawal line. Finned piping is provided to allow use
of carbon steel between the finned piping and the catalyst hoppers. Skin TI’s
are provided upstream and downstream of the finned piping to monitor the wall
temperature of the piping. If necessary, adjust catalyst withdrawal settings to
ensure the skin TI upstream of the finned piping stays below 1000°F (540 °C)
and the skin TI downstream of the finned piping stays below 650°F (343 °C).
4. A large manual operated catalyst withdrawal system is also provided. This

system is used for unit shutdown, or in order to make large changes in the unit
inventory. To operate, open the inboard block valve and start carrying air to the
catalyst withdrawal line. Slowly begin opening the outboard block valve and
adjust the air rate to ensure the temperature on the skin TI stays below 650 °F
(343 °C). If the regenerator pressure is very low, for example during a shutdown,
it will be necessary to pull a vacuum on the equilibrium catalyst hopper in order
to unload the catalyst.
5. Once operations are completed, shut down the outboard block valve first.
Purge the line between the block valves into the regenerator, then close the
inboard block valve. Stem and seat purges are provided to purge catalyst away
from the valves enabling full closure of the valves.
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Figure 4
CONTINUOUS CATALYST WITHDRAWAL SYSTEM
2.5.10 MAIN COLUMN BOTTOMS OPTIMIZATION

Slurry Exchanger Fouling
There are two general types of slurry exchanger fouling: Heterogeneous and
Homogeneous.
Heterogeneous foulant consists of a mixture of small hard coke particles, catalyst and
heavy hydrocarbons. This type of foulant is typically found attached to the tubesheets
blocking the entrance to the tubes. Heterogeneous fouling will result in an increase in
pressure drop as well as a decline in the overall heat transfer coefficient.
One source of the hard coke particles are deposits on the wall of the reactor vapor
line, which have spalled off during a thermal cycle and then carried into the main
column. Therefore it is very important to prevent reactor thermal cycles during
emergencies. Refer to the emergency procedures for instructions on how to minimize
reactor thermal cycles. Note that coke deposits on the reactor vapor line are more
common when processing residual feedstocks.
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Another source of hard coke particles are deposits on the disc and donut trays inside
the main column. These can accumulate if there is insufficient reflux to keep the disc
and donut trays wet. The recommended minimum reflux rate is 6 gpm/ft2 (14.7
m3/hr/m2) of column cross sectional area. These deposits can spall off if the main
column is cooled down during a thermal cycle.
The slurry pumps are provided with basket strainers which are designed to capture
coke particles large enough to block the tube entrance. The baskets should be
periodically inspected and repaired or replaced when damaged.
Homogeneous foulant consists of heavy polynuclear aromatics (HPNA’s) which

deposit as a thin layer on the walls of the tubes. Homogeneous fouling will result in a
decline in the overall heat transfer coefficient with minimal increase in the exchanger
pressure drop. This type of fouling is a complex function of feedstock properties,
catalyst properties, reactor operating conditions and how the main column bottoms
circuit is operated. Homogeneous fouling is also more common when processing
residual feedstocks because these feedstocks have high concentrations of HPNA’s
which are difficult to convert and concentrate in the slurry oil.
Optimization
In many situations, main column bottoms optimization involves maximizing recovery

of LCO while controlling homogeneous fouling. Feedstock, catalyst and reactor
operating conditions are selected based on production goals. Refer to the Normal
Operations section for a discussion on these items. The remainder of this discussion
will be limited to the group of factors associated with the operation of the main column
bottoms circuit. The principal factors which impact homogeneous fouling are bottoms
residence time, bottoms temperature, bottoms composition and exchanger tube side
velocity.
The circulating slurry system is similar to a continuous stirred tank reactor. Some
HPNA’s come directly from the reactor as unconverted feed and concentrate in the
circulating slurry system. Additional HPNA’s are produced within the circulating slurry
system via thermal cracking, and production increases with residence time. A decline
in net slurry oil production will result in an increase in the residence time.
This will occur when operating at high reactor severity or when operating at turndown.
Since the feedrate and reactor severity are set by production goals, the only way to
minimize the residence time is to minimize the bottoms level. The recommended main
column bottoms level during stable operations is 30 %.
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The rate of fouling increases as the tube side velocity decreases. In order to mitigate
fouling, the minimum recommended tube side velocity for slurry exchangers is 4.5 fps
(1.37 m/s). In order to prevent erosion, the maximum recommended tube side velocity
for slurry exchangers is 8 fps (2.44 m/s). Tube side velocity should be calculated based
on the average number of tubes per pass. The flowing density used in this calculation
should be the average of the inlet and outlet density.
The bottoms temperature and composition is a function of the LCO production rate
and the quench oil flowrate. Quench oil is cooled slurry oil from the exit of the steam
generators returned directly into the liquid pool in the bottom of the column. The
bottoms composition becomes heavier and the bottoms temperature increases as
LCO production is increased. However the bottoms temperature can be decreased by
increasing the quench oil flowrate. The maximum recommended bottoms temperature
is 670°F (355°C). As LCO production is increased, the slurry oil composition becomes
heavier regardless of the quench oil flowrate. When the composition becomes heavier,
the viscosity increases, and the potential for fouling increases. The maximum
recommended slurry oil viscosity is 25 cSt at 99°C.
The circulating main column bottoms pumps are rated for 120 % of the normal process
design flowrate. The required quench oil flowrate is difficult to predict, so it is not
accounted for in the normal process design flowrate. However the additional pump
capacity provides for sufficient quench oil to control the main column bottoms
temperature.
Operating Guidelines
Start up the main column along with the reactor and regenerator following the Normal
Startup procedures. The following guidelines should be implemented as quickly as
possible. Do not delay these steps, because fouling will gradually begin as soon as
the unit is on stream.
1. During initial startup and whenever operating at reduced throughput, keep one
of the steam generators on standby. This will allow for lower heat removal from
the column and higher tube side velocity through the operating steam generator.
When the feedrate is increased, bring on the second steam generator.
2. Set the slurry flow to the circulating main column bottoms/raw oil exchanger as
required to maintain the tube side velocity within the recommended guidelines.
The feed temperature is independently controlled by a temperature controller,
which bypasses raw oil around this exchanger.
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3. Set the gross slurry product flowrate through the main column bottoms
product/raw oil exchangers as required to maintain the tube side velocity within
the recommended guidelines.
NOTE: The main column bottoms product spillback valve controls the
gross slurry product flowrate (net plus spillback) through the net slurry
exchangers. The net bottoms flowrate can be independently controlled
by the operator without reducing the tube side velocity through these
exchangers.
4. Maintain a minimum quench flowrate of 10 % of the circulating main column

bottoms pump rated capacity to keep the column internal quench distributor
clear. Increase the quench oil flowrate if necessary maintain a maximum
bottoms temperature of 670°F (355°C).
5. Set the hot reflux flowrate at 6 gpm/ft2 (14.7 m3/hr/m2) of main column cross
sectional area.
6. Adjust the slurry flow to the steam generators as required for main column
fractionation. Maintain the tube side velocities within the recommended
guidelines.
7. Set the main column bottoms level at 30 %.
8. Begin slurry sample collection on a daily basis. Send to the lab and monitor for
specific gravity, viscosity, and C7 insolubles. Adjust the total net LCO flowrate
to maintain the bottoms viscosity below 25 cSt at 99°C.
9. Begin monitoring the slurry exchangers for overall heat transfer coefficient,
tube velocity, and duty.
NOTE: If fouling does occur, it will be necessary to take the exchanger

off line for mechanical cleaning. Once the exchanger is brought back on
line, try to increase the tube side velocity for this exchanger. Additional
flow can be provided by running the circulating slurry pumps at rated
capacity and minimizing the flow through the hot reflux valve (target 3 %
open). Be sure to maintain the total reflux at 6 gpm/ft2 (14.7 m3/hr/m2) of
main column cross sectional area.
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2.6 ANALYTICAL CONTROL PROCEDURE
Refer to Analytical Control Procedure Manual, R2B-P3-206-02-A-MO-00001

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2.7 OPERATING RECOMMENDATIONS FOR

SHUTDOWNS, RESTARTS AND EMERGENCIES
Refer to Operation Manual, R2B-P3-206-02-A-MO-00001

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3. GAS CONCENTRATION
3.1 INTRODUCTION
3.1.1 GENERAL
A Gas Concentration Unit receives gasoline and all lighter products from a Fluid
Catalytic Cracking Unit (FCC) and separates this mixture into stabilized gasoline,
liquefied petroleum gas (LPG), and non-condensable dry gas. The LPG stream may
be further separated into mixed C3 and mixed C4 streams. Gas streams and/or
gasoline streams from other units may also be charged to the Gas Concentration Unit.
An amine absorber for H2S removal is typically installed on the net dry gas stream and
the net LPG stream. Treating units for mercaptan removal are typically installed on the
net LPG stream and the net gasoline stream.
The components in the charge and products from a Gas Concentration Unit are
summarized in the following table:
Component Formula Boiling Point (@ 1 atm)
Gasoline C5+ Hydrocarbons 100 to 430°F (38 to 221 °C)
Normal Butane n-C4H10 31°F (-1 °C)
Isobutane i-C4H10 10°F (-12 °C)
Butylenes C4H8 19 – 40°F (-7 to +4 °C)
Propane C3H8 -43°F (-42 °C)
Propylene C3H6 -54°F (-48 °C)
Hydrogen Sulfide H2S -78°F (-61 °C)
Ethane C2H6 -126°F (-88 °C)
Ethylene C2H4 -155°F (-104 °C)
Methane CH4 -260°F (-162 °C)
Hydrogen H2 -423°F (-253 °C)
Inerts N2, CO, CO2 -321, -314, -108°F
(-196, -192, -78 °C)
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3.1.2 PROCESS DESCRIPTION

Refer to Figure 1. The first step in the Gas Concentration process is the separation of
the non-condensable lean gas from the heavier components. The lean gas can not be
separated in conventional fractionation equipment unless refrigeration is used. A
stripper-absorber system must therefore be used for this primary separation. Net gas
from the FCC unit must first be compressed and cooled before entering the stripper-
absorber system. Typically, a two-stage wet gas compressor is used for this purpose.
The compressor raises the gas pressure and moves the wet gas stream forward for
processing in the stripper-absorber system. A spillback from each stage of the
compressor is provided to prevent the compressor from surging during startup and
unit upsets. The compressor speed is varied to control the FCC main column overhead
receiver pressure.
The heart of a stripper-absorber configuration is the high pressure cooler and receiver.
The high pressure receiver serves as both a surge vessel to dampen process upsets
and as a water settler. All internal streams and all charge streams pass through the
cooler/receiver except for the unstabilized cracked gasoline. Gas from the wet gas
compressor joins the primary absorber bottoms stream, the stripper overhead vapor
stream, and the liquid from the compressor suction drums to enter the high pressure
cooler and then the receiver.
Gas from the high pressure receiver (referred to as rich gas) contains valuable
products in the propane-butane range. The gas is washed with cracked gasoline from
the FCC Main Column Overhead receiver to recover these products in the primary
absorber. Stabilized gasoline is injected at the top of the primary absorber to increase
the C3 and C4 recovery. Heat is generated as the liquid streams flow down the column
absorbing the lighter material from the rising gas stream. This heat is removed via
intercoolers to increase absorption efficiency. The liquid hydrocarbon from the bottom
of the primary absorber is pumped to the high pressure cooler.
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Figure 1
Tropical Gas Concentration Unit
The gas stream from the primary absorber exits from the top and flows to the bottom
of the sponge absorber. The sponge absorber is a packed tower where any remaining
C5+ material is removed by countercurrent contact with a lean oil, specifically Light
Cycle Oil (LCO) from the FCC unit. The lean gas from the top of the sponge absorber
is then sent to an amine absorber for H2S removal. A portion of the untreated lean gas
may be recycled to the reactor riser in the FCC unit as lift gas. The LCO (Rich Oil) is
pumped back to the Main Column.
Unfortunately, absorption is not as selective an operation as fractionation. As such,

the rich oil contains not only the desired C3’s and C4’s, but also a considerable
quantity of the unwanted dry gas (C2-) and hydrogen sulfide (H2S). These
components are removed by charging the high pressure receiver liquid to the stripper.
Reboiler heat is used to strip out the correct quantity of material from the stripper
charge by having the stripper overhead vapor flow reset the reboiler heat input. The
stripper overhead vapor returns to the high pressure receiver and cooler from which
the lighter gases again enter the bottom of the primary absorber.
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The stripper bottoms contains a reduced concentration of C2- and H2S that permits
handling this stream in conventional fractionation equipment. The stripper bottoms
material is separated in the debutanizer into LPG and gasoline. The debutanizer is
operated to control the Reid Vapor Pressure (RVP) of the gasoline product and the C5
content of the LPG product. Heat to the debutanizer reboiler is supplied from
circulating FCC heavy cycle oil. The net LPG is sent to an amine absorber for H2S
removal followed by a treating unit for mercaptan removal prior to the optional C3/C4
splitter. Some of the debutanizer bottoms is recycled to the primary absorber to
increase the C3 and C4 recovery. The remaining net debutanizer bottoms is sent to a
treating unit for mercaptan removal.
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The purpose of the Gas Concentration Unit is to separate gasoline, LPG and dry gas
produced in the FCC Unit. The heart of the Gas Concentration unit is the stripper
column. The purpose of the stripper column is to separate C2- and H2S from the
gasoline and LPG, while minimizing loss of C3 and C4 into the dry gas stream. Note
that since H2S and C2- boil in the same range, it is usually only necessary to monitor
one of these species, usually H2S. The unit is controlled by monitoring the C3 content
of the dry gas from the sponge absorber and the H2S content of the LPG stream from
the debutanizer. In practice, as the C3 content of the dry gas increases, the H2S
content of the LPG stream decreases, and vice versa. For convenient control it is
necessary to observe only one of these concentrations. Typically a Tutweiler buret
(UOP Method 9) or detector tube (Dragger or Kitigawa) is used to determine the H2S
content of the LPG stream and can easily be carried out by the plant operators. Modern
units have an online analyzer on overhead for H2S control. The maximum
concentration of H2S in the LPG stream is usually one of the control points set by the
unit process engineer.
The main operating variable of the stripper column is the stripper overhead vapor flow
rate, which is controlled by adjusting the stripper reboiler duty. This vapor rate is the
primary control in the recovery section of the Gas Concentration Unit. Increasing this
vapor flow will decrease the H2S content of the stripper bottoms but will increase the
propylene and propane content of the dry gas from the sponge absorber. The vapor
flow should be adjusted to give a minimal content of H2S in the debutanizer overhead
(LPG) with a minimal content of propylene and propane in the sponge absorber off-
gas (dry gas).
It is possible to build up a liquid recycle in the absorption section and overload the
stripper and absorbers with liquid. For example, if the stripping rate becomes
excessive, the stripper vapors will contain heavier than desired components that end
up as a liquid in the high pressure receiver. This will increase the feedrate to the
stripper and increase the liquid loading, and consequently, the pressure drop across
the column. These conditions tend to increase liquid entrainment back to the high
pressure receiver magnifying the problem. This may cause liquid entrainment from the
primary absorber into the sponge absorber where it will be returned to the FCC main
column with the rich sponge oil.
The above condition of C3 internal recycle due to overstripping, is easily recognized

by a reduction in the quantity of net gasoline. Levels tend to build in the high pressure
receiver and FCC main column overhead receiver. Also, it is possible to build up a
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cycle whereby the levels in these vessels will continue to build with the pertinent
control valves wide open. The best immediate action to rectify this situation is to
drastically reduce the heat input to the reboiler of the stripper by lowering the setting
on the stripper vapor flow controller until the upset condition is corrected.
A sudden increase in the H2S level of the LPG stream should not be construed as
being a result of lower stripping alone. For example, if the sulfur content of the FCC
Unit charge increases, the H2S content of all the streams will increase in roughly the
same proportion.
Since our objective is to minimize loss of C3 and minimize the H2S content of the LPG
stream, let us examine what variables control the H2S rejection.
3.2.1 LEAN OIL FLOW TO THE ABSORBERS
3.2.1.1 Primary Absorber (DA-21201)
Unstabilized gasoline feed from the FCC main column to the ninth tray of the primary
absorber is not a variable that operators can control. However lean oil (recycled
gasoline from the debutanizer bottoms) to the top tray of the primary absorber can be
increased to increase C3/C4 recoveries. Caution must be exercised to avoid liquid
flooding at high throughputs.
3.2.1.2 Sponge Absorber (DA-21202)
Increasing the lean oil (light cycle oil from the main column) flow rate tends to increase
the absorption efficiency of the sponge absorber. Changes in the lean oil flow rate has
only a slight effect on C3 recovery. The effect is more noticeable on the recovery of
heavier components.
3.2.2 PRIMARY ABSORBER TEMPERATURE
Low temperatures favor absorption, however, absorber temperature is not normally

considered to be a variable. The intercoolers are generally operated at less than 100°F
(38°C). When starting up a Gas Concentration Unit, experienced operators will,
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however, frequently leave the water shut off on the intercooler until the unit is steady
so that H2S rejection is favored. This operation will not scale the coolers because
absorber temperatures are not high enough to precipitate scale from good cooling
water.
3.2.3 HIGH PRESSURE RECEIVER TEMPERATURE
Generally, the high pressure receiver temperature is held close to 100°F (38°C).
Variations of this temperature will result in large variations in the stripping and
absorption rates. Also, the inlet temperature of the hydrocarbon to this cooler is high
enough to scale the tubes should the water flow be restricted.
3.2.4 STRIPPER VAPOR RATE
This is the primary control on the Gas Concentration Unit. Normally all other variables
are held constant and this vapor rate is varied to control the H2S content of the LPG.
3.2.5 SYSTEM PRESSURE
The sponge absorber pressure controller maintains a constant pressure on all vessels
in the Gas Concentration Unit, except the debutanizer. The system pressure is a
secondary control which, though not normally used for day to day operation, can be
used to keep the necessary stripper vapor rate in a convenient range. It may
sometimes be desirable to lower the system pressure when the cracking unit swings
to a high sulfur chargestock because the stripper column will be more efficient.
However, the stripper pressure must always be high enough to charge the debutanizer.
It should also be noted that the absorption efficiency decreases as the pressure
decreases. Thus, more H2S will be rejected, but the LPG recovery will also decrease.
3.2.6 OPERATING VARIABLES
A summary of the operating variables for the Gas Concentration Unit is given below:
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Variable Operating Conditions

Wet Gas Compressor
Speed Automatically adjusted by the main column
pressure controller to maintain column pressure.
Spillback Valves Position Closed during normal operation. Automatically
adjusted by the anti-surge controllers during
startups and unit upsets
High Pressure Recevier
Temperature Floats based on cooling air & water temperature.
Typically 80°- 100°F (27°- 38°C)
Pressure Rides on primary absorber backpressure.
Primary Absorber
Top and intercooler Floats based on cooling air & water temperature.
return temperatures Typically less than 100°F (38°C)
Intercooler flow rates Normally wide open to maximize cooling for good
absorption efficiency.
Pressure Rides on sponge absorber backpressure.
Sponge Absorber
Top temperature Floats based on cooling air & water temperature.
Lean oil flow rate Floats based on cooling air & water temperature.
Pressure Controlled to give good absorption efficiency and

hold correct backpressure on HPR.
Stripper
Overhead vapor flow rate Controlled by heat input to stripper column to give
sufficient C2- and H2S stripping.
Heat input to column Controlled to give proper overhead vapor rates.
Pressure Rides on high pressure receiver backpressure.
Debutanizer
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Tray 10 temperature Controls reflux to give desired RVP of gasoline.
Top reflux temperature Floats based on cooling air & water temperature.
Reboiler heat As required to control C5+ content of LPG
Pressure Varied as needed for good fractionation, but must

be high enough to allow condensation of C3-C4
stream by air or cooling water.
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The Gas Concentration Unit can be divided into two general areas known as the
Recovery Section and the Fractionation Section. In the Recovery Section, ethane and
lighter components and hydrogen sulfide are removed from the feed stream. The
principle pieces of equipment are the wet gas compressor, high pressure receiver,
primary absorber, sponge absorber and stripper. The Fractionation Section in its most
basic form has a debutanizer to split the unstable C3+ products into liquefied petroleum
gas (LPG) and stabilized gasoline.
3.3.1 RECOVERY SECTION
The charge streams to the recovery section of the Gas Concentration Unit consists of
wet gas and unstabilized gasoline from the main column overhead receiver in the FCC
Unit as shown in Figure 1. Small quantities of gasoline or lighter products from other
processes can also be processed in the Gas Concentration Unit.
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Figure 1
Main Column Overhead System
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The wet gas compressor flow and control is shown in Figure 2. Vapor from the
overhead receiver is compressed to above 200 psig (14 kg/cm2) using two separate
stages. The gas is cooled after each stage to remove heat of compression allowing
heavier components to condense out of the gas stream. The gas flows from the main
column overhead receiver through a first stage suction drum to the first stage of the
compressor. The suction drum contains a wire mesh blanket (demister pad) to trap
entrained liquid droplets that could damage the compressor. Any liquid that collects in
the first stage suction drum is pumped forward to the high pressure cooler. The control
system for the wet gas compressor will shut down the compressor on high liquid level
in the first stage suction drum.
The first stage discharge flows through the compressor interstage cooler to the
interstage receiver drum. Wash water is injected to the interstage cooler to prevent the
buildup of salts such as ammonium chloride. The interstage receiver contains a
demister pad to trap any entrained liquid. The liquid collecting in the compressor
interstage receiver (hydrocarbon and wash water) is pumped on level control to the
inlet of the high pressure cooler. The control system for the wet gas compressor will
also shut down the compressor on high liquid level in the interstage drum. From the
top of the compressor interstage receiver, gas flows to the second stage suction of the
gas compressor then on through the high pressure cooler to the high pressure receiver.
The overhead vapors from the stripper, the interstage condensate and the rich oil from
the primary absorber join the second stage discharge gas upstream of the high
pressure cooler.
Both stages of the wet gas compressor are equipped with anti-surge controllers and
spillback valves. During normal operations both spillback valves are closed. If
necessary for unit startup or during a unit upset, the anti-surge controller will
automatically spillback gas to prevent compressor surge.
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Figure 2 Wet Gas Compressor Flow and Control

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Rich Gas flows from the high pressure receiver to the primary absorber for C3/C4
recovery. Refer to Figure 3. The gas flows upward through the primary absorber
contacting a downflow of unstabilized gasoline from the FCC Unit main column
overhead receiver that is introduced into the primary absorber at Tray 9. A slipstream
of stabilized gasoline from the debutanizer is admitted to the top tray of the primary
absorber. The addition of stabilized gasoline to the primary absorber significantly
increases C3/C4 recovery. Off-gas exits the top of the primary absorber and flows to
the bottom of the sponge absorber for final recovery of any C5+ material and some
C3/C4 material. The gas flows upward through the sponge absorber where it is
contacted with a downflow of lean oil which enters the column on flow control above
the packing. The lean gas leaves the top of the sponge absorber on pressure control
and flows to the amine absorber for H2S removal. A portion of the sponge gas may be
recycled to the FCC Unit as lift media.
A slip stream of light cycle oil (LCO) from the FCC supplies lean oil to the sponge
absorber. This lean oil is cooled by heat exchange with rich oil from the bottom of the
sponge absorber and a trim cooler. The LCO is pumped on flow control into the top of
the tower above the packing. The lean sponge oil flows downward through the
absorber contacting the upward flow of gas. From the absorber bottom, the rich oil
(flowing on level control) is heated by the lean oil before returning to the FCC main
column via the LCO pumparound.
Unstabilized gasoline from the FCC main column overhead receiver is pumped on
level control directly to the primary absorber and flows down through the column
contacting the upward flow of gas. Heat of absorption transferred to the liquid is
removed by pumping rich gasoline from the column through upper and lower
intercoolers and back to the column. At the bottom of the primary absorber, the rich
gasoline is pumped on level control through the high pressure cooler and high
pressure trim cooler into the high pressure receiver.
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Figure 3 Absorber
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Liquid hydrocarbon from the high pressure receiver is pumped to the stripper where
hydrogen sulfide (H2S), ethane and lighter components are stripped out. Refer to
Figure 4. Feed to the stripper is heated using the total (recycle plus net) debutanizer
bottoms stream. Stripper charge enters the column above the top tray. Stripping action
is provided via a reboiler at the bottom of the column through which heat is supplied
from the debutanizer bottoms stream and a steam reboiler. Steam flows through the
tube side of the stripper reboiler with its flow regulated by a flow controller that is reset
by the stripper overhead vapor rate. The overhead vapor is returned to the high
pressure condenser. Bottoms material is pressured to the debutanizer on level control.
3.3.2 WATER WASH SYSTEM
The overhead stream from the main column contains various contaminants that may
cause corrosion, plugging or fouling. These include ammonia, sulfides, cyanides,
chlorides and phenols. A wash water stream is used to remove these contaminants
since most are ionic or polar species, and are readily soluble in water. Typical flow
rates are 6 to 7 vol-% of fresh feed, though less may be used if it does the job.
The water should be clean, preferably steam condensate, to prevent adding more
problems such as salts or dissolved oxygen to the system. The water is injected after
the compressor first stage and is pumped out of the interstage suction drum to the
inlet of the high pressure cooler. The water is collected in the water boot of the high
pressure receiver and then pressured back to the FCC main column overhead
condensing system.
There is always water present in the FCC main column and gas concentration section
from reactor stripping stream and other sources. If the wash water is not used to flush
out the sulfides, ammonia, cyanides and other species, the water present can be
highly corrosive from absorption of these contaminants. Sulfide levels of greater than
20,000 ppm have been reported in the overhead receiver water. Hydrogen blistering
and general corrosive attack may become quite severe, especially if feed sulfur is
greater than 1%, or feed nitrogen is greater than 1000 ppm. Also, while the overhead
receiver water may be basic, most of the ammonia that is responsible for this will drop
out in the main column receiver. The water in the gas concentration section may
become acidic from H2S and CN. If there is any oxygen present, elemental sulfur may
be formed from oxidation of the sulfides. This will cause problems in meeting gasoline
product specifications. Wash water will solve many of these problems by diluting the
corrosives and keeping the water pH at 8-9 where sulfide oxidation is greatly reduced.
Refer to Figures 1 and 2. Wash water injected at the wet gas compressor first stage
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discharge flows with the hydrocarbon stream through the interstage cooler, the
interstage receiver, the high pressure cooler and high pressure trim cooler to the high
pressure receiver. The water is collected in the water boot of the high pressure receiver
and is pressured to the Main Column Overhead receiver of the FCC Unit on interface
level control. If needed sour water can be recycled or fresh water can be added to the
main fractionator overhead fin fan condensers.
3.3.3 FRACTIONATION SECTION
As shown in Figure 4, the feed to the Fractionation Section is the stripper bottoms
stream that is pressured into the debutanizer. The debutanizer reboiler uses heavy
cycle oil from the FCC Unit. The HCO is regulated by a flow controller. Overhead
vapors (C3's and C4's) are condensed by an air cooled condenser and then collected
in the debutanizer receiver. Debutanizer feed is preheated by circulating light cycle oil
from the FCC. The net gasoline is pressured from the debutanizer on level control to
a treating unit for mercaptan removal. A recycle stream of stabilized gasoline is also
sent to the Primary Absorber to increase the absorption efficiency of C3/C4.
A portion of the total overhead is pumped back to the column as reflux. The quantity
of reflux is regulated by a FIC which is typically reset by the Tray 10 TIC in the upper
part of the column. The net overhead liquid product is pumped out on flow control that
is reset by the level controller on the debutanizer receiver.
The debutanizer column pressure is controlled by a PIC on the overhead vapor line
and by a PDIC in the vapor bypass line. The PIC controls vapor flow to the condenser
to control the column pressure. The PDIC keeps the receiver pressure from dropping
too low, bypassing some vapor to keep the pressure control valve in range. The
receiver pressure is not always constant and will change with changes in the weather
conditions.
A drag line is provided to vent non-condensables from the top of the overhead receiver.
Column pressure control will not work properly if non-condensables accumulate. If
they do accumulate, first the PDIC control valve will close, then the column pressure
will exceed the setpoint.
The debutanizer overhead product is pumped to an amine absorber and treating unit
for H2S and mercaptan removal.
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Figure 4 Stripper/Debutanizer Flow

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3.4 TROUBLESHOOTING
All UOP operating manuals have a fixed table of contents. As a result, a particular
section may be omitted because it either does not pertain to the operating manual or
it will be presented in another section. The Troubleshooting section is omitted because
it is discussed in the Process Variables section.
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All UOP operating manuals have a fixed table of contents. As a result, a particular
section may be omitted because it either does not pertain to the operating manual or
it will be presented in another section. Any special procedures are noted in Normal
Startup, Normal Shutdown and Emergency Procedures.
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4. CAUSTIC MEROX AMINE SECTION
4.1 INTRODUCTION
4.1.1 GENERAL
The removal of acid gases, such as, hydrogen sulfide (H2S) and carbon dioxide (CO2)
from liquid and gaseous hydrocarbon process streams is desirable for many reasons:
• Safety considerations, to control (reduce) products H2S toxicity
• Environmental considerations, to reduce the sulfur dioxide (SO2) emissions

– acid rain precursor
• Technology enabler, to improve hydroprocessing desulfurization by treating

the recycle gas to increase the hydrogen (H2) partial pressure and reduce the
sulfur load on the desulfurization catalyst
• Product quality improvement:
• Corrosivity reduction, to improve the quality of products, by generally

reducing corrosivity
• Benefits to downstream treating units, to reduce NaOH consumption

since acid gases consume non-regenerable treating solvents
• Energy value improvement, to improve energy value of sales gas by

reducing primarily the carbon dioxide (CO2) content.
To date, the most economical and widely used process for bulk acid gas removal is a
continuous absorption/regeneration process using an aqueous solution of basic amine.
The target acid gases to be removed are primarily H2S and CO2, but other sulfur-
bearing contaminants, to a much lesser extent, may also be removed. These include
carbonyl sulfide (COS) and mercaptans (RSH), when using MEA and DEA. Removal
of carbon disulfide (CS2) is typically so small that no credit is taken for this effect when
using any of the generic amine, e.g. MEA, DEA, or MDEA. It should be noted, however,
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that the removal of mercaptans generally isn’t significant when using MEA, DEA, and
MDEA, and, therefore, usually downstream Merox Treatment or hydroprocessing is
needed. Unfortunately, annoying amounts of other undesirable contaminants may also
be absorbed, such as heavy organics (oil), water, nitrogen, oxygen, salts, mercury,
sulfur, ammonia (NH3) (specially in high nitrogen crudes), hydrogen cyanide (HCN),
etc. These impurities will impact the effectiveness and life of the amine solution.
While the focus of this manual will be on H2S removal, the same principles are
generally applicable to CO2 also. Since both H2S and CO2 are frequently present in
hydrocarbon streams treated by ethanol amines, the term "acid gas" can mean either
or both compounds.
When appropriate, the impact of the co-absorbed impurities will be mentioned. The
names and structural formula for the amines most commonly used are:
Primary amine:
Monoethanolamine (MEA): HO-CH2-CH2-NH2
Secondary amine:
Diethanolamine (DEA): (HO-CH2-CH2) 2NH
Tertiary amines:
Methyldiethanolamine (MDEA): (HO-CH2-CH2) 2NCH3
Proprietary solvents: Based on MDEA with additives
Table I-1 Typical Amine Property Comparison is located on the following page.
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4.2.1 ABSORPTION
The absorption of H2S in the amine solution is favored by:
1. Low absorber operating temperature

2. Proper lean and rich amine acid gas loading
3. High amine concentration
4. High H2S partial pressure in the feed stream
5. Intimate contact between the feed steam and amine
Note: Items 4 and 5 are not true operating variables, having been fixed by the
design criteria for the unit and choice of equipment in the absorber design.
4.2.1.1 Low Absorber Operating Temperature

When treating a hydrocarbon gas the lean amine temperature must be maintained 5-
10°F (3-6°C) higher than that of the gas feed to avoid any possible condensation of
heavy organics (oil) in the amine. The circulating lean amine temperature before it
enters the absorber is commonly between 81 and 120°F max (38-49°C max). These
limits attempt to optimize the amine H2S absorption capacity at practical removal rates;
too low or too high an operating temperature results in poor H2S removal.
When treating a hydrocarbon liquid (LPG) the lean amine temperature is typically
between 100 and 110°F max (38-43 °C max). The lower limit aims to prevent LPG and
amine entrainment and the upper limit is often to prevent poor mercaptan removal in
the downstream treating unit, typically a UOP MeroxTM Extraction Process Unit. The
lean amine temperature should be kept very close to that of LPG to avoid potential
LPG vaporization, especially when the operating pressure is maintained close to the
vapor pressure of LPG.
4.2.1.2 Amine Acid Gas Loading

The rich amine is regenerated to restore the amine solutions capacity in removing H2S
in the absorbers. However, some residual H2S should be left in the lean amine to
suppress corrosion in the lean amine piping and equipment. H2S reacts with the iron
present in the piping and equipment to form a protective iron sulfide film that minimizes
further corrosion; however, the film formed is relatively weakly bonded to the metal
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and requires residual H2S to be present in the lean amine to refresh and sustain the
film.
As the amine descends the amine absorber it becomes increasingly loaded with H2S.
The rich amine loading must be controlled to prevent the forward reaction in Section
II, Equation (4) being hindered and also to prevent the hazard of amine acid gas
breakout that can cause serious corrosion problems after the amine absorber level
control valve. The loading of the rich amine solution is controlled by adjusting the lean
amine flow rate to the individual absorber(s). In most cases, unless special design
considerations have been used, the rich amine acid gas loading (H2S plus CO2) should
not exceed 0.33 to 0.40 mole/mole and the limit depends on the amine being used.
Typical lean amine and maximum rich amine loading guidelines are provided in the
Table III-1.
4.2.1.3 Amine Solution Concentration

The theoretical amine capacity to remove H2S is 1:1; one mole of amine removes one
mole of H2S. Therefore, a higher amine concentration favors higher H2S removal
capacity for the same lean amine flow rate. However, the maximum amine
concentration is limited due to:
• Amine solubility in the hydrocarbon which tends to increase as the amine

concentration increases. Typically, the amine solubility in liquid hydrocarbons
is higher than gas hydrocarbons.
• Amine solution viscosity which increases as solution strength increases.

Increased viscosity reduces the tendency for the amine to disengage from the
hydrocarbon so there is increased chance of amine foaming in gas absorbers,
or emulsions forming in liquid absorbers and entrainment through the amine
process. Circulation (pumping) costs will also increase.
• Amine solution corrosivity which depends also on rich amine loading, but in
general, amine solutions do tend to become more corrosive as amine
concentration increases.
Considering the above points and the cost of amine regeneration, the optimum amine
concentration, confirmed by field experience, is typically between 15 and 45 wt% and
depends upon the type of amine used. Typical amine concentrations are shown in
Table III-1.
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Table III-1
Typical Amine Concentration and Lean and
Maximum Rich Amine Loading
Amine Type MEA DEA MDEA
Primary Amine Secondary Amine Tertiary Amine
Typical Solution 15-20 wt% 20-28 wt% 35-45 wt%
Concentration
Typical Lean Loading 0.07-0.10 0.03 <0.01
(mole acid gas/mole amine)
Maximum Rich Loading 0.33 0.33 0.40
(mole acid gas/mole amine)
4.2.2 REGENERATION
The regeneration of the rich amine, releasing H2S, is favored by:
1. Proper temperature: high in the stripper and low after the condenser
2. Low operating pressure
3. Low H2S partial pressure
4. Proper amine concentration
5. Intimate contact between the amine and stripping steam
Note: Item 5 is not an operating variable and is fixed as part of unit design.
1. Temperature
Amine Stripper Feed

The rich amine feed should be as hot as possible, but not greater than 220°F (105°C)
because of the hazard of acid gas breakout corrosion in the Lean-Rich Amine
Exchanger and after the flow control valve (FCV).
High temperature in the Amine Stripper favors the breakdown of the amine-
hydrosulfide salt into H2S and amine; the reverse reaction of Section II,
Equation (4)
Amine Stripper Condenser

The acid gas formed is cooled to minimize the water losses with the acid gas. However,
there is little benefit cooling the acid gas to less than 95°F (35°C) in gas plant
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applications and less than 115°F (46°C) in refinery applications. High water losses
result in increasing circulating amine concentration and problems in the downstream
treating processes due to the dilution of the amine acid gas by water, which tends to
reduce the H2S conversion potential to elemental sulfur in the downstream sulfur
recovery unit.
Amine Stripper Reboiler

All the commonly used amine solutions begin to decompose at approximately 250°F
(120°C) and the rate of decomposition is becoming excessive at 300°F (150°C). To
minimize and control amine degradation, the typical Amine Stripper bulk temperature
at bottom of the tower is limited to 250-275°F max (120-135°C max), and the reboiler
tube temperature is limited to 325°F max (162°C max).
Note: The amine solutions are mostly water, therefore, temperature changes
with composition are small and it is the operating pressure of the stripper that
predominantly determines the temperature of operation.
2. Low Pressure
The stripper column is operated at the lowest overhead receiver pressure possible
consistent with downstream acid gas processing requirements. Generally, 5 to 15 psig
(35 to 100 kpag) is sufficient pressure to feed the acid gas to the sulfur recovery unit,
or more rarely to an acid gas incinerator.
Note: Lower operating pressure results in lower bulk amine temperature and
lower thermal degradation rates and corrosion rates.
3. Low H2S Partial Pressure

High temperature reverses the reaction shown in Equation (4) and releases the H2S
from the amine. The H2S is stripped by the steam generated in the reboiler. The steam
transfers heat to the amine and reduces the partial pressure of the H2S in the gas
phase, which favors the stripping of further H2S. Normal stripper operations require a
heat input of between 1 to 1.2 pounds of reboiler steam per gallon of amine solution
circulated through the absorber system (120 to 140 kg of reboiler steam per m3 of
amine circulated). Based on experience, this reboiler steam rate will result in a reflux
rate of approximately 3 to 5 LV% of the circulating amine rate.
4. Proper Amine Concentration

The importance of this variable to the satisfactory performance of the unit cannot be
overlooked. If the solvent becomes too dilute, it will not remove acid gas effectively.
Conversely, if the solvent becomes too concentrated, the unit will suffer increased
amine losses, increased corrosion, and increased operating costs, etc. The water
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balance is affected by the following:
1. Dry feed gas will leave the absorber saturated with water, slowly removing
water from the system.
2. Flash gas and acid gas streams will also be saturated with water and thus
remove water from the system.
3. Water is typically purged from the regenerator reflux to prevent the

accumulation of ammonia and other impurities.
4. Makeup water can be added in several ways:
a. One option, rarely practiced today, is to add live steam into the Amine
Stripper Reboiler return line to the Stripper column
b. It can also be added at the inlet of the Amine Regenerator Condenser in

some units, with the added benefit that the water added here acts as a
water wash at this location, and
c. Indirectly, amine rich wash water from the treated LPG Water Wash
vessel (when needed) is pressured into the rich amine line to the Rich
Amine Flash Drum. Note: Due to the relatively high solubility of LPG in
MDEA, a Water Wash vessel is specified to remove this amine from
treated LPG and thereby minimize amine carryover to the downstream
process unit.
Monitoring the solvent water content can also establish the appropriate water purge
or makeup needs.
4.2.3 FEED QUALITY AND RATE
Higher than design feed acid gas content will result in higher acid gas content in the
treated product if the amine circulation rate is not increased to compensate. Likewise,
lower than design feed acid content in the feed could result in excessive stripping if
the amine stripper reboiler duty is not reduced accordingly.
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An increase in the feed gas or LPG rate from the design rate will result in decreased
acid gas removal under the same operating conditions. It could also lead to column
flooding if the feed gas or LPG rate exceeds the operating range of the absorber
internals.
A reduced feed gas or LPG rate may lead to poor flow distribution through the packing
or trays if the rate drops below the operation range of the absorber internals. At lower
hydrocarbon rate, H2S absorption efficiency is reduced drastically. Hence, amine flow
rate is lowered when operating at lower than design rates.
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The actual process flow of a particular unit is specific to that facility. Below is a sketch
of a typical process flow that will be discussed for demonstration purposes.
Typical Flow Diagram for Amine Unit
Single gas and LPG amine absorbers are shown for simplicity. Note that it is more
common for several amine absorbers, gas and liquid type, to be served by a single
amine regeneration unit.
The unit can be divided into five connected sections:

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a. Fuel Gas Purification

b. LPG Purification
c. Amine Circulation
d. Acid Gas Separation
e. Amine Storage and Transfer
The description of each follows:
4.3.1 FUEL GAS PURIFICATION
The sour gas feed enters the Gas Amine Absorber below its bottom tray; there are
typically 10-20 trays (or an equivalent height in packing). The H2S is removed from the
gas by counter-current contact with the amine descending the tower. The purified gas
stream leaves the absorber through a stainless steel mesh demister blanket, provided
to minimize amine entrainment. The purified gas is sent to a Product Knockout Drum
to recover amine entrained with the gas stream.
Sampling connections are provided for the sour gas feed, purified gas, and rich amine
from the Absorber for use in the analysis and control of the absorber operation. The
operating pressure is controlled by a PCV, the lean amine flow to the absorber is
controlled by a FCV, and the rich amine flow from the absorber is controlled by a LCV.
Note that the amine quality is controlled in the amine regeneration section.
4.3.2 LPG PURIFICATION
LPG enters the Amine Absorber on the bottom tray; there are typically 7-10 trays (or
an equivalent height in packing). After contacting the counter current down flowing
amine solution the purified (treated) LPG exits the absorber via the outlet nozzle.
The treated LPG is sent to either an Amine Knockout Drum, to typically recover
entrained MEA or DEA, or to an Amine Water Wash Settler, to recover MDEA, using
a circulating water wash. When MDEA is used for treating LPG streams, a Water Wash
is used to remove the high levels of soluble MDEA in LPG. In Amine Absorber, amine
level is maintained at the bottom of the column.
When LPG Merox unit is not required for downstream processing, treated LPG is sent
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to a Caustic Wash followed by a Sand Filter in order to pass the copper strip corrosion
test. The Caustic Wash is provided to remove remaining H2S sulfur, and the Sand
Filter is provided to remove entrained caustic from the treated LPG.
Sampling connections are provided for the feed, product, and rich amine for use in the
analysis and control of the LPG Absorber operation. The Absorber operating pressure
is controlled by a back pressure controller on the outlet of the Amine Settler or on the
outlet of the Sand Filter. The pressure is set high enough to prevent LPG vaporization.
The lean amine temperature is controlled by the Lean Amine Cooler, the lean amine
flow to the absorber is controlled by a FCV, and the rich amine flow from the absorber
is controlled by a LCV.
Note that the amine quality is controlled in the amine regeneration section.
4.3.3 AMINE CIRCULATION
Lean amine enters the Gas Amine absorbers above the top tray under flow control.
The amine contacts the upflowing hydrocarbon feed gas on each of the trays,
absorbing H2S. The rich amine leaves the absorber through the tower bottom under
level control. The rich amine from the Gas Amine Absorber combines with the rich
amine from the LPG Amine Absorber and flows to the Rich Amine Flash Drum (RAFD).
Rich amine coming from the Gas Amine Absorber and/or Coker LPG Amine Absorber
in the Coker unit should be filtered prior to Rich Amine Flash Drum to remove
particulates. Upon entering the flash drum dissolved gases, light hydrocarbons
(typically C5 and lighter) and unavoidably some H2S, are separated from the amine
and pass upward through a bed of Raschig Rings in the flash drum stack. This flash
gas is washed by a stream of cooled-lean-amine to remove H2S. The amine treated
gases are usually either sent to flare, or more commonly, sent to the refinery fuel gas
recovery system. The RAFD also separates heavy hydrocarbon (typically C6 and
heavier) from the rich amine; the hydrocarbons are usually sent to the slop oil recovery
system under level control. The separated oil at slop recovery system is recycled to
the process units to recover refined valuable products.
Sample connections are provided on the rich amine outlet, and on the gas and liquid
hydrocarbon streams.
Rich amine is withdrawn from the flash drum by the Rich Amine Pumps. These pumps
discharge rich amine to the Amine Stripper through the tube side of the Rich- Lean
Amine Exchanger.
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After passing through the Rich-Lean Amine exchanger, the preheated rich amine
solution enters the amine stripper near the top of the column, typically at tray 3 or 4.
As the amine descends the tower the H2S is stripped through the action of bottom
reboiler. The reboiler uses low pressure desuperheated steam to limit the maximum
tube temperature and prevent amine thermal degradation. The stripper bottoms are
usually reboiled using thermosyphon type amine stripper reboilers. The reboiling rate
is usually controlled by the steam condensate withdrawal using a level controller on
the condensate drum via the condensate pumps.
To control the circulating amine concentration (water balance), makeup water can be
injected into the Amine Stripper receiver.
Lean amine is withdrawn from the stripper bottoms by the Lean Amine Pumps. The
stripper bottoms level is indicated by a level recorder. The Lean Amine Pumps
discharge through the Lean-Rich Amine Exchanger and the Lean Amine Cooler. The
outlet temperature of the cooler is controlled by a temperature controller.
The lean amine then flows to the lean amine filters. The mechanical filters are used to
remove particulates and carbon filters are used to remove hydrocarbons. Typically a
slipstream of 15 – 30 LV% of the total amine is filtered. Flow through the filters is
measured by a flow recorder. Complete valving is provided at each filter unit to allow
online filter cartridge replacement. A sample connection is provided for analysis and
control of the lean amine stream.
After passing through the filters the lean amine flow to all absorbers is controlled by
individual flow controllers, the lean amine flow to the Rich Amine Flash Drum stack is
controlled by a FCV (flow control valve).
Note that the lean amine sent to the LPG Amine Absorber typically passes through a
Lean Amine Trim Cooler in addition to the other exchangers/coolers mentioned above.
This is to avoid LPG vaporization as result of “hot” lean amine.
Connections are provided in the lean amine lines to the absorbers and the discharge
of the rich amine pumps to allow the ad-hoc injection of anti-foam additive as needed.
4.3.4 ACID GAS SEPARATION
The overhead vapor of the amine stripper, typically containing H2S, CO2, water vapor,
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and trace amounts of amine, etc. is cooled in the Amine Stripper Condenser before
passing to the Amine Stripper Receiver. The receiver condensate is refluxed to the top
tray of the stripper through the receiver LCV (level control valve) via Amine Stripper
Reflux Pumps.
Makeup water is injected in the Amine Stripper Receiver to dilute NH3 in the amine
stripper reflux stream as needed. Accordingly, a small purge of reflux water is removed
and sent to the UOP Waste Water Stripper to control the accumulation of NH3, etc., in
the reflux. A high amount of NH3 etc. contributes to corrosion and increases the hazard
of salt formation/fouling of the Lean Amine Cooler. Although the reflux flow is
controlled by the amine stripper receiver level controller, the flow is also measured by
a flow recorder. Adequate stripping is indicated when the reflux rate is maintained near
3 LV% of the total amine circulation. The reflux water circulated to the Amine Stripper
minimizes the amount of amine lost with the acid gases produced. The acid gases exit
the receiver through a stainless steel demister mesh blanket and are usually sent to
either the Claus sulfur recovery unit (commonly a Modified-Claus Sulfur Recovery Unit)
or to the acid gas relief header. Stainless steel piping is used to route acid gases to
Sulfur Recovery Unit. This line may require heat tracing depending upon the H2S and
NH3 content in acid gas to avoid salt formation in stagnant line in case of low
temperature. The acid gas flow rate is measured.
4.3.5 AMINE STORAGE AND TRANSFER
Amine is added and mixed with clean condensate in the amine tank. The solution is
transferred to the amine storage tank and mixed to obtain the operating solution
strength using an amine transfer pump. The tank is provided with a nitrogen gas
blanketing system to prevent oxygen degradation of the stored amine solution. The
amine level is measured by a level indicator.
The transfer pump is piped to take suction from the mix tank, storage tank, or from the
discharge of the lean amine pumps and discharge to the storage tank, lean amine
pumps, or to the suction of the rich amine pumps. The piping has been provided so
that amine can be transferred from the storage tank to the unit or from the unit to
storage.
All low points, equipment, samples, and instrument drains containing amine should be
hard piped to the amine sump to conserve amine. The amine sump is equipped with
a 1 ½ " fuel gas connection to the 3" overhead line to supply a positive pressure to the
sump. The level is measured by a level indicator. Also, the sump is equipped with a
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motor driven pump, which allows the contents of the sump to be transferred to the lean
or rich amine system. The sump pump can be routed to the amine waste drum or truck
system if the contents of the sump tank need to be disposed.
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4.4 TROUBLESHOOTING
Amine Process Unit objective is to achieve the desired removal of the H2S and CO2
while operating in an efficient and safe manner to minimize amine losses and utility
consumptions. There are many factors which can prevent this objective being
achieved. The main factors that will be addressed are:
A. Dirty Amine
B. Foaming
C. Failure to Meet Design Specifications
D. Corrosion
E. Amine Losses
4.4.1 DIRTY AMINE

Dirty amine is both a symptom and a cause of amine system failures. Circulating
contaminated amine will eventually curtail the ability of the unit to achieve adequate
acid gas removal. Investigating the condition of the amine can reveal several relevant
indicators of operating trouble. Contaminated and “dirty amine” is indicative of poor
and troublesome operation. Visibly contaminated amine can also tend to be corrosive.
Determining the causes of contaminants build up and what can be done to clean up
the amine is discussed below.
• Some typical symptoms of a dirty, corrosive amine system are:

• Carry-over of amine from the scrubbers
• Dilution of the amine system with water due to reboiler leaks
• Plugging of instruments taps with particulates in the amine
• Loss of amine to the sewer because of leaks
• Rich amine leaking into lean amine in the Rich-Lean exchanger
Checking and troubleshooting of the unit is required if any of these symptoms are
observed.
The investigator performing troubleshooting should first draw a sample of lean amine
into a glass container and visually assess its condition. The visual results can be
rated as follows:
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Amine Visual Inspection:
Bright and Clear: Quality of amine is good. Water white or straw color is normal.
Tea Color: Tea color or light orange/brown and translucent is indicative of thermal
degradation.
(Emerald) Green: Emerald green and translucent is indicative of light corrosion.
Dark Brown: Dark brown and much less translucent is indicative of heavy
corrosion.
Black: Light watery black show polish is indicative of extremely heavy corrosion.
White Coffee Like: White coffee is indicative of corrosion and dissolved

hydrocarbon.
Turkish Coffee: Dark black non-translucent watery fluid and accumulation of black
sediment on bottom of sample is indicative that amine is severely fouled with
suspended solids.
Other colors:
Water White with Hydrocarbon Layer: This is indicative that Skimming is required.
Translucent with Blue Tinge: This is indicative of presence of cyanide. These

cyanides will promote corrosive failures in the amine regenerator overhead system
and, hydrogen blistering or cracking in piping and vessels that contact the lean amine
can occur if hydrogen is present.
Sampling Amine
A sample of unfiltered lean amine should be submitted to the lab to determine
quantitatively the wt% of particulates. Amine solution should contain less than 0.01 wt%
particulates. Sampling should be done using the vendor sample kits for shipment and
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full analysis including heat stable salts. The heat stable salts, which are dissolved
contaminants, should be <1 wt% in total.
Cleaning the Amine
Inadequate filtering will result in an accumulation of particulates and other

contaminates in the circulating amine solution. The amine filtration system treats a
slipstream of cooled lean amine using a combination of mechanical filtration and
activated carbon. The mechanical pre-filter removes particulates from the amine that
would otherwise plug the carbon filter. The carbon filter absorbs heavy hydrocarbons
or soluble materials that have contaminated the amine. The effluent from the carbon
filter passes through the mechanical post-filter to remove carbon fines/particulates
before the slipstream of lean amine is returned to the circulating amine.
At least 10-25% of the circulating amine should be filtered on a continuous basis.

Although filtering a greater proportion of the amine does tend to keep the circulating
amine in the best condition, it also results in the highest consumption of mechanical
filter cartridges and activated carbon as well. For a clean unit, changing the
mechanical filter cartridges each month is normal. When the amine is very dirty
(brown/black), the cartridges may need changing more frequently, for example, every
day for a month, or more, before the circulating amine condition is improved. Cartridge
change out can be scheduled using the mechanical filter DPI (Differential pressure
indication). The lifespan of an activated carbon depends on the amount of dissolved
contaminants in the amine and the flow rate of amine through the filter. While the
expected life of most carbon beds is 3 to 4 months, or greater, system upsets will
shorten the carbon life. Excessive use of anti-foam also reduces the carbon filter life
because the active ingredients are absorbed by the carbon bed.
To properly clean the amine, the rate of particulate generation must be less than the
rate that the particulates can be removed by mechanical filtration. Increasing the
filtration slipstream and changing the cartridges more frequently can help remove the
particulates.
The following guidelines can be used to determine when the carbon bed is
approaching the end of its active life:
• No color change across the filter or darkening of the amine solution color. As
the carbon bed is spent and contaminants begin to build in the solution, the
bulk solution color will begin to darken. If the solution color is dark, but there is
noticeable improvement in color across the bed, the carbon is still active.
Likewise, if there is no color change across the bed but the solution color and
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clarity are good and Fe level is low, then the carbon is probably still active.
• High pressure drop exists across the bed. Carbon beds generally do not show
an increase in pressure drop, as they absorb contaminants with little change
in pressure drop unless there is particulate fouling of the bed. Should this occur,
a backflush may permit continued operation.
• The start of, or increase in the foaming tendency of the amine carbon bed inlet
compared to outlet indicates possible chemical saturation of the carbon and
time for it to be changed.
Spent carbon beds require reloading with fresh activated carbon if backflushing does
not restore adequate activity. Note that some customers have attempted to regenerate
the activated carbon using steam stripping, but the results of this procedure can be
variable. In addition, steam stripping introduces new hazards that must be managed
such as:
• production of waste vapor and effluent process streams
• exposure of equipment to high temperatures, and
• potential damage of activated carbon bed/equipment due to relatively low

ignition temperature of active charcoals, etc.
4.4.2 FOAMING
Clean amine doesn’t foam. The presence of contaminants in circulating amine

increases the foaming tendency. Contaminated amine tends to form stable amine
foam (gas treating applications) or stable amine emulsions (liquid treating application)
that cause upsets. Depending on where the foam/emulsion (“foaming”) is formed,
foaming may upset the operation of the Amine Absorber, Rich Amine Flash Drum,
Regenerator, etc.; therefore, amine foaming can result in off- specification product
streams, reduced operating rates, significant amine losses, and possible
contamination of downstream processes.
Detection
Foaming upsets can cause the following:

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• Oscillation in pressure drop across a column

• Sudden increase in acid gas removal followed by a swift drop in removal
• Unexpected level changes in the tower or other vessels
• Amine carryover from Absorber, Regenerator or Rich Amine Flash Drum
• Off-specification treated gas
• Positive results from foam test
• Poorly stripped solvent
A foam test should be performed on a sample of lean amine often. A nil or slight
foaming tendency requires no action. Moderate or severe foaming tendency may
require the addition of anti-foam.
Causes of Foaming
Typical causes of foaming are contaminants that cause the amine to be dirty. These
components act to reduce the surface tension of the circulating amine
promoting stable foams. Consistent filtering and reclaiming can control most of these
problems. Each typical cause is discussed below.
Corrosion inhibitors can cause foaming. The impact of any corrosion inhibitors or
other additives should be tested individually. Pour some freshly made amine solution
into a clean bottle. Add a typical concentration of the inhibitor or additive and conduct
the foam test to record the foaming tendency. Trace amounts of these chemicals can
cause foaming so include additives/inhibitors in the investigation even if they are
added significantly upstream of the amine unit.
Anti-Foam Agents (silicone, polyglycol or high Molecular weight alcohols) can cause
foaming when used in excess. A batch dose of antifoam will temporarily stop foaming,
but too much will make the problem worse. Antifoam usage should be considered a
temporary treatment while the root cause(s) is identified and corrected. Use the
appropriate antifoam recommended by UOP for the plant’s application.
Carbon filters need to be changed. Several percent of the circulating solution should
be passing through a carbon bed. The carbon removes surfactants. Change the
carbon when it is spent, and do not let carbon fines enter the regenerator and
scrubbers, as these fines also cause foaming. For further information about how to
forecast when a Carbon Filter change out is needed, see Cleaning the Amine in the
DIRTY AMINE section above.
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Particulate Filters (usually cartridge-type) should be replaced on a regular basis to

keep amine solution visibly free of particulate matter. See also Cleaning the Amine in
the DIRTY AMINE section above.
Hydrocarbons in Solution: Gas-phase hydrocarbons will condense in the amine

solution, if the lean solvent temperature is below the feed hydrocarbon dew point. The
lean amine temperature should be 3 - 5 ºC above the dew point of the feed
gas. Cooler amine will condense liquid hydrocarbons and trigger foaming. Liquid
hydrocarbons entrained with the feed gas can enter the system and cause foaming if
inadequate inlet separation exists. Other sources of hydrocarbons are upstream
process lube oils or process chemicals, pipeline corrosion inhibitors, etc. Note that a
lean amine – hydrocarbon feed temperature differential is not required in liquid- liquid
treating (e.g. the LPG Amine Absorber).
Detergent cleaners may have been used during a unit turnaround. When the unit is
put back on-line, the detergent finds its way into the amine system. The carbon filter
should absorb this detergent. Before the startup of the amine unit, the unit should be
flushed via several water rinses. The rinse water should be checked for neutral pH
and foam tested for nil foaming tendencies to assure that all of the soap/detergent has
been removed.
Solvent Properties: Like most fluids, the viscosity of amine solvents will increase as
the temperature decreases. As viscosity increases, the tendency for the fluid to
support foam will also increase. A change in viscosity can be caused by over cooling
the lean solution, or allowing the solvent concentration to exceed recommended
maximum concentration guidelines, or by over cooling the inlet gas.
In Summary foaming can be reduced or controlled by proper care of the amine

solution and by the following techniques:
1. Knock-out drum upstream of the gas absorber to minimize liquid hydrocarbons

and iron sulfide/suspended particles and well-treating chemicals from entering
the amine system
2. Proper clean-out of new equipment prior to start-up and proper rinsing
3. Adequate carbon and mechanical filtration and maintenance
4. Proper operation to minimize amount of hydrocarbon contamination in amine

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5. Proper operation to minimize corrosion
6. Routine foam testing of lean amine before and after the carbon filter, routine
foam testing of makeup water, and processing additives interaction with
samples of the circulating lean amine solution
7. Temporary use of antifoams on an as-needed basis while the root cause(s) is

identified and corrected
8. Use of the UOP recommended antifoam for the application
4.4.3 FAILURE TO MEET DESIGN SPECIFICATIONS

Any changes in operating conditions, unexpected upsets, foaming, corrosion, or amine
losses may result in the failure to meet design specifications. The following is a list
of possible causes and conditions to check and troubleshoot if there is a failure to meet
design specifications.
1. Changes in feed acid gas content: If the inlet gas acid gas concentration
increases then more moles of acid gases must be removed to meet the given
specifications. Daily monitoring of the acid gas content of the feed is part of
our analytical schedule recommendation so that such changes are observed.
Providing more moles of amine to accommodate the increased removal is the
typical course of action. Roughly, an acid gas increase to 110% of design may
roughly need circulation rates of 110% of design rate. Operating up to 110%
of the design circulation rate is usually comfortably within the operating
margins of the equipment and the hydraulic capacity of the columns.
Operation above 110% of design capacity, the product may go off-spec unless
other conditions favorable to absorption are also adjusted. However, if
expected on a sustained basis, debottlenecking assessments may be required
to handle the increased removal demand.
2. Changes in feed gas temperature:
a. If the feed gas temperature has become hotter than expected, it may be
above the gas dewpoint which could enable condensation of liquid
hydrocarbons in the Absorber column if the gas drops in temperature
while passing through the column. Setting the lean solution temperature
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to be incrementally higher in temperature could offset this, but absorption

performance will be reduced by hotter temperatures.
b. If the gas is too cool, the solvent contacting it will also drop in temperature
and increase in viscosity. Higher viscosity solvent hinders efficient mass
transfer and therefore affecting the ability to meet specification.
3. NH3 content in feed gas: When NH3 is present in the feed gas, NH3 will get
absorbed in amine solution and routed to Amine stripper along with rich amine.
This NH3 finally accumulates in amine stripper reflux circuit and higher amount
of NH3 can lead to ammonium bisulfide (NH4HS) salt formation. These salts
can cause fouling in trays and exchangers/reboiler. To reduce the NH3
concentration in reflux circuit, dilute the reflux with wash water and purge out
extra sour water from reflux to the sour water stripper unit.
4. Lean amine solution temperature too high: Absorption is favored by cooler

lean amine temperatures, therefore the solution should be cooled to the design
temperature unless it is kept hotter to assure being above the gas dew point
to avoid hydrocarbon condensation.
5. Fouled lean/rich exchanger and/or lean amine cooler: Fouled exchangers

inhibit effective heat transfer that results in a cooler rich solution to the
Regenerator and a hotter lean solution to the cooler and Absorber. Poor heat
transfer in the lean amine cooler leads to poor absorption as mentioned in item
#2 above. The cooler rich solution requires that more thermal energy be
supplied to the reboiler to satisfy the higher sensible heating demand (higher
temperature delta from the rich inlet temperature to the boiling point of the
solution) in addition to heat of vaporization (boiling) requirement. If the heat
input is manually controlled and is not reset, then the solution may not be
properly regenerated. Note also that the amine stripper is designed to be
operated so that the majority of the acid gas stripping occurs in the upper
section of the tower. If however, the rich amine feed temperature is too cold
this will tend to result in more acid gas stripping in the lower part of the tower,
where operating temperatures are higher and corrosion due to this cause (mal-
operation) can be serious.
6. Lean/rich exchanger by-pass opens too far: Same impact as mentioned in

item #5 above.
7. Higher than design circulation rate: If the circulation rate is too high the
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Absorber may be hydraulically over-loaded which can lead to flooding.
8. High ambient temperature: If air coolers are used for lean solution and acid
gas cooling then, in the case of the lean solution, the lean temperature to the
Absorber will be higher with the impact as described in item #2 above. If the
acid gas is not cooled to the design expectation, then less water will be
condensed from the solution which could affect the availability of the reflux
water for return to the column. This would result in a higher water loss in the
acid gas and may require an increase in the makeup water requirement.
9. Low Amine concentration: Low concentration will result in less moles of

amine available for each mole of H2S and CO2 to react for loading into the
solution and removal by regeneration.
10. Lean loading too high: Too high loading is an indication that the solution is
not being efficiently regenerated. The system should be checked for the
following likely causes and steps taken to correct them.
a. Insufficient stripping steam in Regenerator

b. Low/high-Regenerator pressure
c. Foaming in Regenerator
d. Contaminated/dirty amine solution
e. Poor contact in Regenerator due to circulation rate below minimum
column turn down rate
f. Factors affecting proper contact in Regenerator such as fouled,
plugged, or damaged internals (trays or packed beds)
11. Plugged or fouled trays or packing in Absorber: Solids and various other
deposits and precipitates can plug and foul Absorber internals (trays or
packing). This interferes with the necessary contact of vapor and liquid for
proper mass transfer. It also causes poor distribution on the internals surface
and may increase the delta pressure (DP) through the tray or packed bed.
The increased DP can also lead to amine carryover.
12. Lean Amine circulation rate too low: Similar to item #9 above, a low
circulation rate, even at the design concentration of the solvent, may not
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provide enough moles of amine for reacting and loading with the moles of H2S
and CO2.
13. Absorber Gas pressure has dropped: The higher the absorption pressure
the higher the partial pressure of the contaminant component as a driving force
for loading into the solution. If the pressure drops, then the driving force for
H2S removal is reduced.
14. Absorber operation below minimum turndown: There is a minimum

turndown rate below which mal-distribution of flow across a packed bed or tray
weeping can occur. The poor contact that result from the poor hydraulics
causes a loss of absorption efficiency.
15. Operation above the maximum gas: Operation at high gas to liquid ratios
that exceed the hydraulic maximum may trigger flooding. The poor contact as
a result of the poor hydraulics causes a loss of absorption efficiency.
16. Degraded solvent or HSAS (heat stable amine salt) build-up: The
absorption efficiency is affected by solvent quality and availability of free amine
moles. There are less moles of active amine available for acid gas removal
when the solvent degrades. The solvent may have degraded due to an
oxidation reaction (oxygen ingress in the system) or excess reboiler heat
(thermal degradation). Solution purging and makeup or reclamation may be
required if the HSAS continues to increase past the 1 wt% maximum.
17. Mechanical damage: Damage to the internals in the Absorber or Regenerator

will interfere with proper contact and mass transfer and can result in flow
blockages, high column DP (differential pressure), and flow channeling. Poor
Mechanical damage can occur in the regenerator due to the following:
a. Collapsed trays/broken packing

b. Plugged and/or broken distributors
c. Corrosion
Checking for damage symptoms may reveal this. Other methods, such as
tower gamma scanning, can be used to determine the type and location of
internal damage.
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18. Foaming (Refer to Part B. Foaming in this Section)
19. Contaminated/dirty amine (Refer to Part A. Dirty Amine in this Section)
4.4.4 CORROSION
Fresh amine solvents are not corrosive, however, the processing environment can be
corrosive due to the presence of carbon dioxide, H2S, chlorides, heat stable amine
salts (HSAS), etc. which act as corrosive agents. The possibility of two-phase flow in
pipes, when acid gases flash from solution present additional possibilities for corrosion.
High particulate concentrations, especially if combined with high solution velocities,
introduce the hazard of erosion-corrosion. These effects, especially if occurring at the
same time, can lead to rapid metal loss. Therefore, effective corrosion prevention
depends on proper operation and dealing with the contaminants that cause corrosion.
To address this, stainless steel is used in the areas where very high corrosion rates
are expected. However, there are carbon steel areas where corrosion may occur due
to conditions that are outside the expected operating range, or in cases where self-
forming inhibiting layers, such as the iron sulfide layer formed by H2S and carbon steel,
is disturbed by a physical factor (e.g. erosion). Understanding the corrosion
mechanism and typical symptoms and causes enables better effort in troubleshooting
and minimizing corrosion.
Mechanism of corrosion by acid gases
Carbon dioxide reacts with water vapor to form carbonic acid, which readily attacks
mild steel. The iron carbamate formed does not form a passivating film and cannot
prevent further attack. However, H2S reacts with iron to form a film of iron sulfide, FeS,
which inhibits further reaction and protects from corrosion. The reaction is as follows:
The formation of the passifying iron sulfide film alters the metal surface to halt further
corrosion by H2S. When over-stripping occurs in the Regenerator, there will be
insufficient H2S to form the passivating film, and therefore the overall susceptibility of
the unit to corrosion will increase.
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Chloride contamination often results in stress corrosion cracking of stainless steel.

Chlorides are typically brought into the system via:
• poor quality make-up water, or

• entrained with the hydrocarbon feed, or
• Introduced by water cooled exchange leaks (if applicable)
Heat stable amine salts, HSAS, precursors are organic acids like formate, acetate,
thiocyanate, etc. The HSAS’s are formed by the reaction between the amine and the
corresponding acidic contaminant such as formic acid and acetic acid that may enter
with the feed. These amine salts are called heat stable because they cannot be
(thermally) regenerated, to release the bound amine, under normal Regenerator
temperatures. HSAS tend to dissolve the protective iron sulfide film, exposing the
metal to further corrosion, and also form Fe-complexes resulting in reduced treating
capacity. Corrosion from high HSAS concentration is usually limited to the hot areas
of the system: reboiler tubes, lean/rich exchanger tubes, and hot lean piping.
Areas of highest corrosion potential
The areas with the highest corrosion potential tend to occur in areas of high acid gas
loading, high temperature or both. Unusually high levels of contaminants such as heat
stable amine salts, or particulates combined with high solution velocities tend to cause
higher rates of corrosion. The indications or symptoms that corrosion is occurring
include:
1. High solution metals (Fe, Cr, Ni, etc) content

2. High concentrations of heat stable amine salts
3. High total suspended solids (causing erosion/corrosion)
4. Wall thinning using ultrasonic monitoring
5. Physical leaks
6. Vessel Failure
7. Positive solution corrosivity test
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Figure X–1 indicates the principal areas where corrosion can occur in the Amine
Process Unit.
FIGURE X–1
Areas of Corrosion Potential
Common types of corrosion in amine units are:
1. Stress corrosion cracking of stainless steel is often the result of chlorides that
are introduced to the system from poor quality makeup water or entrained with
the feed gas.
2. Sulfide stress cracking is a type of spontaneous brittle failure in steels and

other high-strength alloys when they are in contact with moist H2S such as in
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flashed.
3. gas from the Rich Flash Drum or after pressure let-down and entry of rich
solution into the top of the Regenerator.
4. Erosion can be caused by a high amount of particles in solution in areas of

high solution velocities and changes in flow direction such as pump impellers
and piping bends.
4.4.5 AMINE LOSSES

There will be a certain amount of amine lost in the normal operation of the Amine
Process Unit. However, excessive losses, beyond the normal level, are a very
common and costly problem. Amine losses are generally controllable and can be
minimized by good design and operation. The principal causes of amine losses are:
- solvent carryover from entrainment, foaming and amine solubility in

hydrocarbons
- Leaks from equipment, seals, etc., due to corrosion, poor maintenance, etc.
Specifically, Amine losses occur by four key means outlined below.
1. Mechanical losses are any permanent, unwanted or unscheduled physical

removal of solvent from the plant. This can occur due to:
a. Leaks at pipe/flange gasket connections

b. Pressure gauge/sample line purges
c. Un-rinsed cartridge filter elements
d. Amine sump contamination/disposal
e. Heat exchanger leaks
f. Pump seal flushes or leaks
g. Frequent filter changes
h. Un-rinsed carbon bed
i. Excessive daily sample volumes
2. Entrainment losses are when unwanted or uncontrolled gas-in-liquid

dispersions (foams) are formed. This can occur due to any of the following
reasons:
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a. Tower pressure below design

b. Trays at or above flooding
c. Amine distributors plugged
d. Damage knock-out vessels
e. Trays damage or plugged
f. Damaged or missing mist eliminator
3. Vaporization losses involve higher-than-expected levels of amine in gaseous

or mist form that leave with the exiting sweet/treated gas. This can occur if the
amine concentration is higher than design, if the system temperature is too
high or if the system pressure is lower than design. The temperatures of the
column overhead areas (especially the regenerator which operates hot) may
be particularly susceptible to this type of loss.
4. Degradation of the Amine contributes to losses because degraded solution is

no longer effective at acid gas removal. Solution monitoring that considers the
“effective” amine concentration can track the degradation losses. Degradation
of the solution can occur due to the following.
a. Chemical degradation resulting from a reaction with oxygen or an oxidizing

agent
b. Thermal decomposition that occurs in reboilers as a result of tube skin
temperatures that are greater than maximum design specification
c. Heat stable amine salt formation. These salts can form via reactions with
inlet gas contaminants or by oxygen degradation or by thermal
degradation of by-products
Guidelines for minimizing Amine losses
Having a better understanding of four typical causes that result in amine losses, the
following guidelines should be followed or implemented.
1. Minimizing Mechanical losses
a. Check the units for mechanical leaks and provide good maintenance to
prevent them.
b. Avoid taking unnecessary large volumes of sample and excessive line
purging.
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c. Care should be taken that flow-through to flare type sample lines are not
leaking or left open. Same with low point drains or liquid sample points to
open or closed sewers.
2. Minimizing Entrainment losses
a. Check the amine content and purge and makeup the water loop to
maintain efficient amine washing.
b. Monitor and maintain demister pads.
c. Monitor the liquid level in the treated gas knock-out drum for excessive
carryover.
d. Control and prevent foaming in the unit to avoid carryover of solvent
e. Maintain gas velocities below maximum hydraulic limits of the Absorber to
prevent solvent droplets from being forced out with the treated gas
3. Minimizing Vaporization losses
a. Cannot be avoided but they tend to be small

b. Implement or improve a water wash system
c. Maintaining reboiler and lean solution temperatures below maximum to
prevent vaporization of solvent
4. Minimizing Degradation losses
a. Regularly monitor solution quality and heat stable amine salt content via
analytical testing by the plant lab.
b. Avoid thermal degradation by maintaining solution temperatures below the
130 C maximum.
c. Provide inert gas blanketing on amine storage tanks (fresh and
circulated amine)
d. Avoid oxidizing agent exposure
Following these guidelines and practices will minimize all Amine losses.
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UOP recommends that specific procedures are obtained or developed for:
• LPG Amine Absorber tray leak testing (see below for UOP guidelines).
• Vendor guidelines for particulate filter and carbon filter operation.
• Amine reclaiming equipment. Amine reclaiming equipment is usually provided

if MEA is used, otherwise no specific equipment is usually provided and
instead periodic amine reclaiming is scheduled using the amine analysis
results.
• Cleaning of the amine unit. Specific guidelines for amine unit cleaning aren’t
provided in this manual, because the method will depend to a large extent on
the local requirements.
See Section VI, Commissioning, for special degreasing procedures required for amine
units.
This section covers the following procedures that are specific to the Amine Process
Unit:
A. Leak Test Instructions

B. MEA Reclaiming
C. Charging the Solvent
D. Hydrocarbon Skimming
E. Antifoam Addition
F. Carbon Bed Maintenance
4.5.1 LEAK TEST INSTRUCTIONS
These instructions are for leak testing the inlet and outlet weirs (downcomers included)
on the LPG amine absorber. It is recommended that the leak testing be conducted
initially on the lowest tray and then on each subsequent upper tray. All tray manways
need to be removed for the leak test.
1. Check the level on the weir top edge. The edge should be level. Repair or
adjust the level as necessary per the specified tolerance.
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2. Tightly plug the downcomer with a blind plate and neoprene gasketing.
3. Plug the inlet weir weep hole if one exists with a plug, cloth, plastic, or other
suitable material.
4. Starting with the bottom trays, carefully fill the inlet and outlet weirs to
approximately ¼” from the top of the weir plate with water. This can most
conveniently be done with a long hose with an on/off valve at the end. Try to
minimize the spillage outside of the weir pans to avoid the amount of drying
required.
5. Thoroughly dry all areas of the tray and vessel shell underneath the outlet and
inlet weir pans using cloths or an air hose. This will allow any leaks present to
be very easily identified.
6. Check all weld points:
• On the downcomer,
• Where the downcomer connects with the outlet bottom pan,
• Along all edges of the inlet and outlet weirs, both above and below the tray
(weir sides, weir pan bottom, edges immediately above and below the tray.
7. Note that no leaks, dripping, seeping or sweating is allowed! Mark any of

these defects for repair with a crayon or chalk.
8. Unplug the downcomer and the weir weep hole to drain all the water.
9. Repair any and all leaks found as marked per UOP recommendations. Repeat
from Step 4 upon the completion of the repairs until no leaks, dripping, seeping
or sweating are evident.
10. Remove the downcomer blind plates.
11. Ensure that the trays are clean of all debris and/or dirt before proceeding with
closing the tray manways. (Note: When installing the tray manways, verify that
the tray manways are correctly installed so that the specified equilateral pitch
is maintained across the manway and tray.) A one-piece neoprene gasket
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should be used for the tray manways.
4.5.2 MEA RECLAIMING
4.5.2.1 BACKGROUND
Reclaiming is a general term for any method by which a solvent is liberated from a
chemical complex formed by a chemical reaction that is "irreversible" under usual
operating conditions. Because the reaction is "irreversible", the solvent is non-
regenerable and no longer functions in the normal manner in the cyclic absorption/
regeneration process. In reclaiming, the solvent complex is subject to special
treatment and another chemical reaction that frees the solvent when a different
complex is formed. The freed solvent is then separated from the newly formed
complex and returned back to the process.
Specifically, this discussion will deal with reclaiming MEA solutions using sodium
carbonate to free MEA from its complexes and permit it to be distilled back into the
process.
The incentives that dictate the inclusion of an amine reclaimer in the amine treating
unit are threefold.
a. Solvent Losses
The extent to which the MEA is irreversibly tied up is directly dependent upon the
quantity of reactive contaminants in the hydrocarbon being treated. Those
contaminants that irreversibly form heat stable amine salts are SO2, NO2, O2, HCl,
cyanides, and carboxylic acids. Effective removal of these compounds can be realized
by water washing prior to amine treating. However, trace quantities that do enter the
amine system will cause continuous consumption of available MEA. The cost of
continuously replacing the MEA must be compared to the capital and operational costs
of an amine reclaimer.
b. Solvent Corrosivity
As mentioned earlier, the presence of O2 will convert aminehydrosulfide to thiosulfate.

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The presence of O2 in the hydrocarbon will also convert MEA to glycine and oxalic
acid. These compounds when present in a CO2 saturated amine solution make the
solution corrosive toward iron. The dissolved iron drops out of solution in the amine
stripper when the CO2 is stripped from the amine. These corrosive compounds
continue to circulate with the amine causing additional corrosion. Therefore, a small
quantity of O2 contamination can cause a persistent corrosion problem in the reclaimer.
The sodium, present as sodium carbonate, will convert these corrosive compounds to
their respective sodium salts and remove them from the system.
c. Foaming
The accumulation of non-regenerable substances such as carboxylic acids in the

amine solution can result in foaming in the stripper and gas absorbers and emulsions
in the liquid/liquid absorbers. In all cases, the result is entrainment and subsequent
loss of the amine solution with the LPG from the absorbers or with the acid gas from
the stripper. Operation of the amine reclaimer on a constant basis will eliminate a
buildup of non-regenerable substances in the amine solution.
4.5.2.2 PROCESS FLOW
The reclaimer resembles a kettle-type shell and tube reboiler. A small cylindrical vapor
disengaging area is connected vertically to the exchanger shell to improve vapor flow
returning to the stripper. Heating steam flows through the tubeside of the exchanger
on pressure or flow control while condensate is removed by a float-type steam trap.
Initially, the shellside is inventoried with sufficient soda ash to provide a 3 wt-% solution
within the reclaimer. A slipstream of the circulating lean amine is fed to the shellside
on reclaimer level control, with the level set to assure that the exchanger tubes are
always submerged. As the temperature rises, vapors are generated and returned to
the amine stripper to supplement the stripper reboiler duty. The temperature in the
reclaimer will initially rise until the molar composition of the vapor returning to the
stripper is identical to the lean amine feeding the reclaimer. See Figure XIII-1. This
temperature is generally 250-270°F (120-130°C) depending on the stripper operating
pressure. In time, the soda ash within the reclaimer becomes consumed, as it forms
sodium salts with acids, and liberates MEA. This will be evidenced by a further
temperature increase in the reclaimer liquid. When the reclaimer temperature rises to
a predetermined maximum, about 300°F (150°C), the reclaiming operation is
temporarily suspended.
Thus, reclaiming operation is a semi-continuous/batch operation. The sodium salt

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residue must be periodically discarded and fresh soda ash charged to the reclaimer.
The reclaimer is equipped with a live steam sparger and a treated water connection,
attached to the bottom of the exchanger shell, to facilitate the removal of the spent
soda ash. These same facilities also assist in the maximum recovery of MEA prior to
the reclaimer shutdown for recharging.
The MEA reclaimer is designed to be constructed of standard materials and to be

easily cleaned. No brass, bronze, or copper bearing alloy is used where it will come in
contact with the amine liquid or vapor. Only iron or steel is incorporated in the reclaimer
fabrication.
4.5.2.3 RECLAIMER OPERATIONS
The reclaimer operations are categorized as:
a. Initial Startup
b. Normal Operations
c. MEA Recovery
d. Cleaning
a. Initial Startup
1. Check that all instrumentation is checked and made operational.
2. Verify that the reclaimer utilities are in services such as: Steam Supplies,
Condensate Header, and Treated Water Supply.
3. Visually inspect the reclaimer internals for general cleanliness. Wash out
any foreign matter that may have collected during construction.
4. Add sufficient powdered soda ash (Na2CO3) to provide a 3 wt-% solution

in the volume of amine present at a normal operating level above the
steam bundle. The soda ash should be charged through the smaller
loading flange located on the top of the horizontal portion of the reclaimer
(typically 10").
5. Verify that the soda ash is well dispersed up to the loading flange within
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the shell and head.
6. Fill the reclaimer shell with lean amine via the level control valve to a level
8 to 12 inches above the tubes. Put the level controller in service.
7. Commission the tubeside steam and condensate removal systems and

slowly increase the steam pressure control to 100 psig (690 kPa). Monitor
the reclaimer shellside pressure.
8. When the reclaimer shellside pressure increases to the same pressure

present in the amine stripper bottom, slowly open the gate valve in the
reclaimer vapor return line.
9. Verify that the shellside level controller is operating properly and begin
recording the reclaimer liquid temperature.
b. Normal Operations
1. Lean amine is charged to the reclaimer by the level control valve

maintaining a liquid level above the tubes. Periodically, any amine present
in the amine sump can be pumped directly to the reclaimer. The lean
amine slipstream should be approximately 3-LV% of the total amine
circulation rate.
2. If the reclaimer tubeside steam flow is pressure controlled, adjust the

steam pressure to maintain the specified lean amine makeup rate. This is
usually done incrementally as makeup flow starts to fall off. If the steam
flow is flow controlled, adjust the steam flow to maintain the specified lean
amine makeup rate.
3. As the amine solution boils, water vapor initially passes from the reclaimer
concentrating the MEA. The MEA solution in the reclaimer will concentrate
to about 70 wt-% MEA at which point the vapor in equilibrium with this
liquid will contain 20 wt-% MEA. This is equal to the concentration of the
entering lean
4. amine liquid; therefore, the concentration ceases and the reclaimer liquid
temperature will stabilize at about 270°F (130°C), depending on stripper
bottoms pressure.
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5. As MEA is being liberated from complexes and leaves behind heavier

sodium salts in the reclaimer liquid, the boiling point of this liquid gradually
increases. When the reclaimer temperature reaches 300°F (150°C), the
MEA itself will begin to decompose unless the procedure is stopped. At
this point, the lean amine makeup is stopped and the MEA recovery
operation begun.
6. If excessive reclaimer temperature is suspected, take a reclaimer vapor

sample through a sample cooler and observe its color. The condensed
sample should be clear and nearly colorless, similar to fresh, lean amine.
c. MEA Recovery
1. To avoid decomposition and loss of the reclaimer liquid which is 70 wt-%

MEA, the reclaimer liquid temperature must be restricted to a maximum of
about 300°F (150°C).
2. The lean amine makeup on level control is discontinued and treated water
is used to maintain the reclaimer level. The water will dilute the MEA
concentration and allow the MEA to distill at a lower temperature. The
reboiler steam rate should be reduced to minimize excessive dilution in
the stripper during the ensuing operation.
3. Live steam is introduced via the sparger in the bottom of the reclaimer.
These vapors aid in stripping the MEA from the liquid and increase MEA
recovery.
4. Water makeup and stripping steam are continued and the reclaimer liquid
is periodically sampled and analyzed for X MEA.
5. It is normally not economical to try to continue the MEA recovery

operations when the MEA content of the reclaimer liquid drops below 5 to
8 wt-%.
6. To stop the MEA recovery operations:
a. Discontinue reclaimer steam flow to the reclaimer tubeside.

b. Block in the makeup treated water.
c. Discontinue the live steam to the sparger.
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d. Block in the reclaimer vapor line isolating the reclaimer from the amine
stripper.
e. Depressure the reclaimer shell and open the vent.
d. Cleaning
1. Following the MEA recovery operation, drain the remaining sludge from the
reclaimer to the oily water sewer. Quench the draining with any convenient
water source.
2. Use the water connection and live steam sparger to rinse out and clean the
reclaimer internals.
3. Continue flushing the reclaimer to sewer until the effluent water is clear.
4. Open the soda ash charging flange and visually inspect the reclaimer tubes
for cleanliness. If deemed necessary, the tubes can be further cleaned
manually with steam or high pressure water.
5. Reload the reclaimer with fresh soda ash proceeding as outlined in the initial
startup instructions.
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Figure XIII-1
MEA Reclaimer
Vapor-Liquid Curve for Aqueous Monoethanolamine Solutions

Pressure 10 psig (69 kPa)
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4.5.3 CHARGING THE SOLVENT

The amine solvent must be charged before entering the system. This is done as
follows:
1. Estimate the volume needed to maintain proper levels in all the major vessels
(drums, columns, etc.) and the liquid-filled volume in other equipment such as
exchangers as well as the major process piping.
2. Calculate the amount of pure amine that is needed to achieve the desired
design concentration of solution when mixed with water.
3. Add around 80% of the pure amine volume calculated according to item #2
above to the amine storage tank and add water to dilute to the required
concentration.
4. Begin to circulate the solution. Add more amine and water, as necessary, to
achieve the normal working levels in vessels and requirement amine
concentration. Note that some more solution will be required to maintain liquid
levels in vessels during hydrocarbon processing, because some solution will
be held up on trays or packing within the columns.
5. Analyze the cool solution for desired concentration of solvent. Final mixing of
two hours should ensure a uniform mixture.
Note that solution preparation can also be done prior to charging to the unit if a solution
makeup/preparation tank is available.
4.5.4 HYDROCARBON SKIMMING

The removal of hydrocarbon from the Absorber sump and the Rich Amine Flash Drum
will be discussed separately. Note that UOP does not have detailed procedures for
these operations. The following outline is provided as a guideline for the
contractor/client to develop their procedures. Ensure that appropriate safety measures
are reviewed prior to implementing the procedure.
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4.5.4.1 Absorber
Hydrocarbon can collect on the top of the gas/amine interface in the sump section of
the Absorber. Often this layer can be emulsified and is referred to as the rag layer.
Decanting of the rag layer from the Absorber is a manual operation. The design of the
Absorber column includes a skimming nozzle located above the normal liquid level. If
a rag layer is suspected, operations must increase the level in the sump up, so that
the liquid level is just above the skimming nozzle. The operator then should slowly
open the skimming line valve. Care must be taken to avoid gas breakthrough.
4.5.4.2 Rich Amine Flash Drum
The Rich Amine Flash Drum is designed as a three-phase separating vessel to enable
removal of any liquid hydrocarbons into the hydrocarbon section of the drum. The
baffles have been designed to allow for hydrocarbons to build up to a level where they
would overflow into the hydrocarbon section. Once a sufficient level builds up, the
high alarm will sound, indicating that the hydrocarbon section needs to be drained.
The material drained should be handled in the same manner as skimming operation
from the absorber. Hydrocarbon is drained to the closed drain sump. Any recovered
amine solvent is then drained to amine sump.
4.5.5 ANTIFOAM ADDITION

A variety of solvent contaminants can lead to foaming including liquid hydrocarbons,
incompatible additives such as corrosion inhibitors, high levels of suspended solids,
and high heat stable salts, among others. The suspended solids in treating solutions
can lead to erosion in the system which further escalates the solids level in the system
and may also promote or stabilize any existing foam tendency of the solution.
Moderate or severe foaming tendencies can inhibit proper mass transfer and lead to
other operating problems and carryover. To address foaming issues, antifoam addition
is required.
Antifoam addition is generally not required in amine units and thus is not
recommended for continuous use. However, it is recommended for use as a temporary
solution to stabilize the system until the root cause of the foaming is determined and
addressed. During pre-commissioning, it is recommended that a baseline
concentration of 200-300 (max.) ppm of the total inventory be charged to the
circulating solution before processing gas. Before charging the antifoam a foam test
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should be completed with a sample of amine to confirm compatibility.
There are several antifoam types such as silicon-based. Higher boiling alcohols like
glycols are not recommended as glycol foam sometimes deposits in the unit. The
silicones are commercially available either as water emulsions or in their pure form.
The most applicable antifoam type is usually determined on a plant by plant basis. As
a general statement, silicones are sometimes found to be effective in gross foaming
situations where antifoam, that can more significantly alter surface tension properties
and break the foam, is required.
Antifoams are usually added batchwise when needed. The Antifoam injection station
details are given in UOP Schedule A specification.
The typical stream locations for antifoam injections as shown in Figure XIII – 2 are:
• Lean solution inlet line to the Absorbers

• Suction of the Rich Amine Pump
Figure XIII – 2
Typical Antifoam Injection Points
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4.5.6 CARBON BED MAINTENANCE

1. De-aerating
In a volume of 283 liters (10 ft3) of carbon there is approximately 113 liters (4 ft3) of
void space, 113 liters (4 ft3) of pore volume and 57 liters (2 ft3) of skeleton carbon. If
the carbon is not properly de-aerated prior to startup, roughly 40 percent of the bed
volume will remain occupied by air. Air must be judiciously removed from granular
activated carbon before a bed is put on stream since the oxygen will react with and
degrade the amine solution.
The following data indicate that the time required to pre-wet or de-aerate activated
carbon is a strong function of temperature.
Carbon and/or Water Carbon and/or Water Time to be 95%

Temperature (ºF) Temperature (ºC) Wetted
70 21 3 Days
212 100 3 Hours
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De-aeration of the carbon can be accomplished as part of the bed loading procedure.
The bed is loaded hydraulically with carbon/water slurry or with dry carbon.
5. Loading
Wet Loading
Carbon is added to water or fresh solution in a vessel or drum and allowed to stand
prior to the filling of the adsorber. When wetting of the carbon is essentially complete,
it is then dumped, pumped or pressurized as slurry into the adsorber vessel. When
pumping, provisions should be made to maintain an adequate carbon-liquid ratio in
the transport line (0.45 kg carbon per 3.79 liter liquid or one pound carbon per gallon
liquid). When the bed has been filled with slurry, there will be an excess of water.
Therefore, the product discharge valve must be opened or an overflow arrangement
made to discharge the excess liquid during the loading operation.
Dry Loading
In the dry loading procedure, the adsorber filled with one quarter full of water or fresh
amine at as high a temperature as is safe. One quarter of the total carbon charge is
then added and allowed to stand until 95 percent wetted. If possible, the bed is then
backwashed with H2O or fresh solvent at a rate of 2.4 - 9.8 m3/hr/m2 (1 -
4 gpm/ft2) for 5 - 10 minutes. Another one quarter addition of carbon is made, allowed
to stand, and then backwashed. This procedure is repeated until the bed has been
filled.
After the adsorber has been filled with carbon, the bed should be backwashed by
introducing hot water into the bottom of the column at a rate of 1.2 - 2.4 m3/hr/m2 (1/2
- 1 gpm/ft2) of bed cross-sectional area for 1 - 2 hours. This procedure will remove any
fines which may have been created during handling, plus air pockets that may have
been trapped in the bed. During backwashing, the flow rate should be controlled so
that the carbon bed does not expand to the point where the particles classify (bed
stratification).
6. De-Fining
It is desirable to remove as many fines as possible from the carbon bed prior to start
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up. Elution of carbon fines into the main circulating solution is the primary cause of
system foaming when a new carbon bed is commissioned. The procedure described
for de-aerating carbon in the adsorber will also de-fine the carbon, provided the water
overflows during the backwash step.
When the carbon bed is brought on stream, the water occupying the void spaces
(approximately 40 percent of the bed volume) should be routed to sewer. During this
step, a quantity of fines will be removed from the adsorber. In general, this is the end
of the elutriation of fines during an adsorption cycle. However, if the bed is upset by
an abrupt pressure swing or viscosity increase, more fines may come out of the bed.
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Figure XIII – 3
Carbon Bed Back Flush For Particulate Matter Removal
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7. Discharging
As a safe practice the bed should be purged to atmosphere to remove H2S prior to
opening the filter housing. If the spent carbon is to be collected by the manufacturer,
the solution occupying the filter should be displaced from the bed using one or two
bed volumes of cold water. This water and solution can be returned to the system so
that no waste water results from preparing the carbon for collection.
Granular carbon can be discharged by gravity alone. A 20 percent volume of liquid in

excess of the liquid which fills the void space is required for carbon to flow freely from
the adsorption column. This implies that roughly 610 mm (2 feet) of water above the
carbon should be maintained during discharge of approximately 2400 mm (8 foot)
carbon filter.
The contaminants adsorbed on the carbon may have vapor pressure and boiling points
which are higher than the temperature of the available steam, so it is often impractical
to regenerate the bed.
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5. CAUSTIC MEROX LIQUID/LIQUID

EXTRACTION
5.1 INTRODUCTION
5.1.1 MEROX PROCESS OVERVIEW

The UOP Merox Process is an efficient and economical catalytic process developed
for the chemical treatment of petroleum distillates for removal of sulfur present as
mercaptans (Merox Extraction) or conversion of mercaptan sulfur to a less
objectionable form (Merox Sweetening). The process relies on UOP developed
catalyst, specifically designed to accelerate the oxidation of mercaptans to disulfides
at economical product rundown temperature.
The Merox process is based on the ability of a catalyst composed of iron group metal
chelates to promote the selective oxidation of mercaptans to disulfides in an alkaline
environment, using air as the source of oxygen. This technique has long been known
but was generally impractical without a catalyst. It was not until UOP introduced Merox
catalyst in 1958 that the great economic advantage of regeneration of caustic by use
of atmospheric oxygen was fully realized (see Figure I-1).
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Figure I-1
Oxidation of Mercaptans with Air and Caustic
The reaction proceeds at an economically practical rate at normal temperatures for

refinery rundown streams. For liquid stocks, operating pressure is controlled above
the bubble point to assure liquid phase operation. Downstream pressure requirements
are easily taken care of by use of appropriate size product pumps.
Merox treatment can, in general, be utilized in the following ways:
1) Odor improvement on all stocks.

2) Reduce sulfur content of products to meet specifications for motor fuel or other
combustion processes.
3) Reduce sulfur content of FCC, coker or visbreaker C3/C4 olefins resulting in
decreased acid consumption during alkylation operations using these
materials as feedstocks.
4) Meeting the requirement of low sulfur for sensitive catalyst used in various
chemical synthesis processes.
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5.1.2 MEROX ADVANTAGES
Relative to other treating processes, the Merox Process has the following advantages:
1) Low operating cost and investment requirement. The initial investment in many
applications can be very low based on the conversion of existing equipment
for use in Merox Treating processes and minimal plot area requirement. Low
utility and chemical usage result in low operating costs.
2) Ease of operation. Merox Process Units are simple to operate; the air injection
rate is the only direct adjustment necessary to accommodate wide variations
in feed rate or mercaptan content. Operating labor requirements are minimal.
3) Proven reliability. The Merox process has been widely accepted by the
petroleum industry; over 1800 units of various kinds (extraction, liquid, and
fixed bed sweetening) have been placed in operation.
4) Minimal chemical disposal requirements.
Proven ability to produce on specification products. There is no product deterioration

due to side reactions or need for addition of undesirable materials to the treated
product.
5.1.3 HISTORY OF THE UOP MEROX PROCESS
The 1500th UOP Merox Unit started initial operations on October 19, 1993, currently
there are over 1800 units in operation across the world.
The remarkable popularity of the UOP Merox process around the world is unrivaled by
any other petroleum refining process and very few oil refineries are in operation
without one or more Merox Units to treat the products. The popularity of the UOP
Merox Process can be attributed to its economical operation, ease of control, and
ability to chemically treat mercaptans in a manner unique to Merox.
The basic Merox patents were issued to UOP researchers W. K. T. Gleim, et al. in the
late 1950's and early 1960's. The manager of the UOP Treating Department, Kenneth
M. Brown, saw the myriad advantages for the Merox catalyzed mercaptan oxidation
over the other available processes and set out to convince UOP management to
commercialize the process. At this point in time, the major treating processes in
commercial use were:
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Caustic Extraction/Steam Regeneration – for gas streams, LPG and light gasoline
Caustic Scrubbing/Inhibitor Sweetening – for FCC and light thermal gasoline
Copper Chloride Sweetening – for low mercaptan feedstocks
Doctor Sweetening – for high mercaptan feedstocks
Having spent 20 years trying to develop procedures to understand and overcome the
shortcomings of these processes, Ken Brown is credited with developing and molding
the research work into a viable, economical, commercial refinery process which we
today call "Merox".
During the 1960's, UOP continued to improve the Merox process and its application to
the treatment of LPG (extraction), FCC and light gasolines (liquid-liquid sweetening),
and kerosene and jet fuels (fixed bed sweetening). In the early 1970's, changes in
FCC Unit operations led to the development of the Minalk version of the fixed bed
sweetening process. The first extraction unit treating a mercaptan rich gaseous
methane stream was put in service in 1976. In the same year, two, relatively new,
easy-to-use Merox catalyst were commercialized and an entirely new catalyst for
sweetening kerosene feed stocks was created.
In 2001, customers were given the option of using the Extractor Plus™ design. The
new design combines the functions of the Caustic Prewash, Extractor, Caustic
Knockout Drum and Sand Filter vessels into one column. The use of a multifunctional
column reduces unit plot area and results in a reduction of the initial investment cost
for the unit. Other features of the new design are: continuous caustic prewash
circulation, caustic heater and oxidizer outlet temperature control, continuous Merox
catalyst injection, and improved handling of the spent gas stream.
In 2010 UOP released the design of the Disulfide Scrubber. The new lean caustic
wash oil system greatly reduces the disulfide content in the lean caustic. The packed
bed column achieves this by counter current contact of the lean caustic against the
wash oil phase. Application of this technology allows ultra-low product sulfur
concentrations of less than 1 wppm to be achieved.
In 2013 UOP introduced the Enhanced Prewash Section for H2S, CO2 and COS
Removal, located at the bottom of the Extractor Plus column. The hydrocarbon
feedstock enters the bottom section of the prewash after being contacted with a
circulating aqueous mono- or di-ethanolamine [MEA or DEA] and NaOH solution for
COS removal. The COS present first reacts with the MEA to release H2S which is then
quickly absorbed by the sodium hydroxide. Any H2S present in the hydrocarbon will
also be removed in this section.
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In 2014 UOP released the MVP Regeneration design: This Modular Equipment
offering optimizes the design of the traditional Merox caustic regeneration section
redesigning to reduce the size and number vessels required. This results in plot space
reduction of more than 25% when compared to the conventional regeneration design.
Upgraded technology of the MVP Regeneration includes all the benefits of the disulfide
scrubber for ultra-low product sulfur while simplifying operation and improving safety
by reducing the volume of spent air by 25% and sulfur emissions by more than 90%.
Over the years, the UOP Merox process has revolutionized the refining industry in the
chemical treatment of petroleum products. It is UOP's constant aim to improve and
simplify the Merox process and to educate our licensees in its application. There was
a time when treating was an art, not a science, practiced in the far corners of the
refineries by people long suspected of possessing magical rather than technical skills.
Today there exists a sound logical understanding of chemical treating which needs
only to be put into practice.
The distribution of operating Merox Units by type is approximately:
Extraction 32%
Extraction + Sweetening 12%
Minalk Fixed Bed Sweetening 14%
Kerosene and Jet Fuel Sweetening 42%
Table I-1 illustrates the applications for treating the various streams via the Merox
process.
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Table I-1
Applications of the Merox Process
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5.1.4 GENERAL TREATING TERMS

Azeotrope a mixture of substances that behaves as a single substance in
that the vapor produced by partial evaporation has the same
composition as the liquid.
Antioxidant chemical additive to inhibit oxidation reaction
Barrel 42 U.S. gallons measured at 60°F
BPD barrels per day (also BSD)
Caustic sodium hydroxide solution
C/H caustic/hydrocarbon volume ratio
delta P (dP) differential pressure
delta T (dT) differential temperature
disulfide class of sulfur compounds characterized by a sulfur-to-sulfur

bond and relatively low volatility represented by the general
formula RSSR
EP endpoint (ASTM distillation)
Enhanced Current design configuration that removes H2S, CO2, and COS
Prewash from the hydrocarbon prior to extracting the mercaptans
Extraction removal of mercaptan sulfur from hydrocarbon
Extractor Plus™ current design configuration of the extraction version of the Merox
process. A caustic prewash section for H2S removal, a mercaptan
extraction section, and a coalescing section to remove entrained
caustic are integrated into one column.
GC or GLC gas chromatography
Gph U.S. gallons per hour
Gpm U.S. gallons per minute
Gum polymerized hydrocarbon

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hydroperoxide compound responsible for propagation of gum forming chain

reaction (-OOH)
IBP initial boiling point (ASTM distillation)
Inhibitor compounds responsible for delaying or terminating a chemical

reaction
LHSV liquid hourly space velocity
mercaptan common name given to class of compounds having thiol

functional groups represented by the general formula RSH
Merox® Process a UOP licensed process that uses a metal based catalyst to
oxidize mercaptan sulfur to disulfide oil
MVP Current regeneration design configuration that accomplishes all

of the regeneration section operations in 2 vertical vessels,
minimizing vessels and plot space
naphthenic acid organic (carboxylic) acid
Nm3 normal cubic meter (1 atm. 0°C)
std. m3 standard cubic meter (1 atm. 15°C)
organo-metallic complex compound characterized by weak carbon to metal

bonds
ppm parts per million
PW prewash
re-entry sulfur entrained disulfide sulfur in regenerated caustic that enters and
dissolves into the exiting hydrocarbon product from an extractor
RX reactor
SCFH standard cubic feet per hour (1 atm. 60°F)
sweetening conversion of mercaptan to disulfide without desulfurization
Stability quality of a fuel to remain unchanged for long periods of time in

storage
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Thiol sulfur-to-hydrogen bond
thiophenol common name given to aryl mercaptans; also the compound

C6H5SH
vol., vol% volume, volume percent
vppm volume (mole) parts per million
wt., wt% weight, weight percent
wppm weight parts per million

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5.1.5 CHEMICAL ABBREVIATIONS AND SYMBOLS

A• inhibitor free radical
C carbon
C1 hydrocarbon with 1 carbon atom (e.g., methane)
C2 hydrocarbon with 2 carbon atoms (e.g., ethane)
Cn hydrocarbon with n carbon atoms
CaCO3 calcium carbonate
CO2 carbon dioxide
H hydrogen
H2S hydrogen sulfide
Na sodium
NaHS sodium bisulfide
Na2CO3 sodium carbonate
NaOH sodium hydroxide (caustic)
Na2S sodium sulfide
NaSR sodium mercaptide
Na2S2O3 sodium thiosulfate
O oxygen
O2 diatomic oxygen (normal form in gaseous state)
R- alkyl group side chain
R• alkyl free radical
RSH mercaptan
RSSR disulfide
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S sulfur
S° elemental sulfur
-SH thiol (mercapto functional group)
unsaturated cyclic hydrocarbon compound
saturated cyclic hydrocarbon compound
[] solution concentration (moles/liter)

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This section discusses the major Merox process variables and their effect on
performance. Specific emphasis will be placed on identifying the optimum operating
conditions. The following represent the five primary process variables. Each will be
discussed as an independent with all others held constant.
C atalyst
O xygen
A lkalinity
C ontact
H eat
5.2.1 CATALYST CONNENTRATION
The extractive Merox process requires the use of UOP Merox Reagent WS-2. It is
supplied as a dark blue solution packaged in 2 U.S. gallon (7.6 liter) sealed
polyethylene bottles. Alternatively, Merox WS-2 can be supplied in 55 U.S.-gallon
drums and 330 U.S-gallon IBC containers.
Catalyst will be further discussed in the Regeneration GOM.
5.2.2 OXYGEN INJECTION
Oxygen is supplied to the caustic regeneration section of the Merox Unit in the form of
compressed atmospheric air. The amount of excess air injection is highly dependent
upon the individual feedstock, but normally ranges between 1.2 to 2.0 times the
theoretical requirement.
Oxygen injection will be covered in the Regeneration GOM
5.2.3 ALKALINITY
Alkalinity is provided by aqueous sodium hydroxide, or caustic, solution. Other

synonymous terms include caustic soda and lye. In this manual “caustic” is the generic
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term used. Caustic is the solvent provided for mercaptan extraction and also the
medium in which the catalyst is dispersed. In addition, it provides the alkaline
environment necessary for the mercaptan oxidation reaction to proceed.
For mercaptan extraction, 20° Baume (14.4 wt-% or 4.15 g-mol/liter) caustic is the
optimum concentration for dissolution of the light mercaptans present.
For low molecular weight mercaptan molecules, (methyl and ethyl mercaptan),
increasing caustic strength increases extraction. As higher molecular weight
mercaptan molecules are encountered, increasing caustic strength decreases
extraction as shown in Figure III-. An upper limit of 25° Baume (19 wt%) is the
maximum practical concentration. Above this strength, competition from the hydroxide
ions already in solution hinders any increase in mercaptan solubility. Also,
emulsification problems begin to occur at these strengths.
Figure III-2
5.2.4 CONTACT
Contact may be defined as mixing intimacy of the reactants and is accomplished by

one of several means. Contact can be characterized by duration of mixing time,
volumetric ratio of phases, or differential pressure. Differential pressure is directly
related to the degree of dispersion. With a fixed flow restriction, the differential
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pressure is directly related to the linear velocity.
For liquid/liquid extraction units, hydrocarbon tray hole velocity is one of the variables
with which contact is characterized. The optimum hole velocity (Figure III-) is designed
for each unit based upon the intended design feedstock. As hole velocity decreases,
extraction efficiency decreases. However, the lower extraction efficiencies at turndown
rates are compensated by higher caustic to hydrocarbon ratios obtained by
maintaining a constant net caustic rate to the top of the extractor.
Figure III-3
UOP Merox Extraction Tray
Overall Efficiency
The other important contact variable for extraction is the volume of caustic circulated
relative to the volume of hydrocarbon throughput. This is referred to as the caustic to
hydrocarbon ratio (C/H). As this ratio is increased, contact is increased and the
extraction potential is increased. Increased extraction occurs as a result of a favorable
shift in the complex equilibrium conditions discussed earlier.
To increase the C/H ratio at constant hydrocarbon feed rate, the caustic circulation
rate must be increased. Any entrained disulfide oil remaining in the regenerated
caustic as it enters the top of the extractor is completely extracted by the exiting
hydrocarbon stream (see Figure III-).
Sulfur in the Merox product as a result of this effect is referred to as re-entry sulfur
(Error! Reference source not found.). At a constant feed rate, re-entry sulfur increases
in the treated hydrocarbon in direct proportion to the caustic circulation rate increase.
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Figure III-4
Re-entry Sulfur
Since increasing the caustic to hydrocarbon ratio increases re-entry sulfur

proportionally and decreases mercaptan sulfur exponentially, there exists a single
optimum ratio where total mercaptan sulfur plus re-entry sulfur is minimized (see
Figure III-5). Above the optimum C/H ratio, increased re-entry sulfur can be excessive;
below it, mercaptan sulfur extraction may be inadequate.
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Figure III-4
Optimum Caustic
5.2.5 HEAT (TEMPERATURE)
Mercaptan extraction is favored by lower temperature. The lowest practical

hydrocarbon feed temperature for extraction is about 90°F (32°C). Below this
temperature, caustic entrainment, or caustic haze, may become a problem. Above
110°F (43°C) mercaptan extraction will be lower and may cause excessive
temperatures in the regeneration section. Extraction Merox Units operate best within
a temperature range of 90 to 100°F (32º-38°C).
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5.3.1 PROCESS FLOW
The basic Merox process unit consists of 3 main sections: Caustic Prewash, Extractor,
Caustic or COS Settler and a Sand Filter or a Water Wash as stand-alone vessels.
The general flow scheme for the hydrocarbon section follows this sequence:
Feed contacts caustic to remove H2S and CO2 in the Prewash. Subsequently,
mercaptan rich feed enters the Extractor bottom tray and mixes with mercaptan rich
caustic from the upper trays. Rich caustic exits the bottom of the Extractor and flows
to the regeneration section while hydrocarbon flows up through trays, counter-
currently extracting mercaptans with caustic. Regenerated (lean) caustic enters at the
top tray of the Extractor, setting the equilibrium concentration by contacting the
hydrocarbon with the least amount of mercaptan with the leanest caustic. The
hydrocarbon stream exits the vessel and flows downstream to a Caustic Settler or an
optional COS Solvent Settler, and a Sand Filter or an optional Water Wash before it
leaves the unit. This can be seen in Figure IV-1.
Figure IV-1
Merox Extraction Unit
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While the original Merox configuration is still available as a less preferred option, the
Merox unit design has many options that improve on the basic design and add to
the flexibility of the unit to treat many types of feed contaminants. By adding or
modifying parts of the process various product quality specification can be met.
Pretreatment:
The Pretreatment section may contain an Amine Absorber Column, which is included
in the scope of the Amine Absorber GOM. The Merox Pretreatment section originally
consisted of a Batch Caustic Prewash, but other options include:
• Batch Caustic Prewash

• Continuous Caustic Prewash (Standard Offering now)
• Enhanced Prewash (H2S, CO2 and COS)
° No Trays for low COS
- Feed contacts a solution of amine and caustic across a static mixer

to remove H2S, CO2, and COS. Solvent is continuously circulation
and made up either batch wise or continuously.
° Trays for High COS
- Same as no tray system, except some of the solvent circulation is

directed to the top tray for more contact and removal.
• Extractor Plus Bottom Section – Any of the above prewash styles can be
incorporated into the Extractor Plus.
Extraction:
The Extraction section has remained basically the same throughout the years with
high velocity jet deck trays providing contact for the phases. However design
improvements have led to the development of the state of the art Extractor Plus™
column, which is the current standard offering. The options are:
• Conventional Extraction Column

• Merox Extraction Plus Column (Standard Offering)
° This configuration stacks the continuous Caustic Prewash and Extractor

vessels to form the bottom two portions of the column. The top section of
the column has been extended to form a disengaging zone to replace
the Caustic Settler followed by a Coalex Coalescer located at the top
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of replace the Sand Filter. This can be seen in Figure IV-2
Post Treatment:
The Post-Treatment section has many optional configurations to meet various product
specifications for sales and internal downstream technology usage. These include:
• Caustic Settler - Remove bulk caustic carryover

• COS Removal Section
° Continuously circulation vessel with a static mixer to provide contact

between the COS solvent and the hydrocarbon to remove wppm COS to
1 wppm amine. Batch make up and withdrawal of amine, caustic, and
water solution.
• Water Wash – Batch or Continuous
° Remove caustic and amine as requested by the customer when

downstream users are sensitive to caustic and amine requiring caustc
below 1 wppm.
• Acidified Water Wash
° Trayed vessel using an acidified water solution to remove all basic

chemicals from the hydrocarbon solutions. Used for nill caustic or amine
downstream
• Sand Filter – used for less than 1 wppm Na+ downstream of the process
• Extractor Plus Top Section – (Standard Offering)
° The top section of the column has been extended to form a disengaging
zone to replace the Caustic Settler followed by a Coalex Coalescer
located at the top of replace the Sand Filter.
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Figure IV-2
Merox Extraction PlusUnit
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1. Pretreatment
Hydrocarbon feed with objectionable levels of H2S flows to the Batch Caustic Prewash.
In the traditional configuration, this is a separate vessel upstream of the Extractor and
is typically operated batch-wise. Streams containing less than 100 wppm of H2S can
be treated in this section.
Hydrocarbon feed containing H2S, CO2 and COS flows to the Enhanced Prewash.
With Extractor PlusTM technology, the prewash is the bottom section of the column
where H2S and COS is removed from the feed stream by a continuously circulating
solution of caustic and amine called COS solvent. The COS solvent from the bottom
of the Enhanced Caustic Prewash section is pumped into the incoming feed, contacted
across a static mixer or mixing valve, and circulated back to the prewash section where
hydrocarbon and COS solvent separate.
The continuous COS Solvent circulation provides better mixing of the hydrocarbon and
caustic resulting in better H2S and COS removal than the conventional batch system.
Streams containing less than 200 wppm of H2S can be treated in this section.
Enhanced Prewash removal of COS is achieved by adding primary or secondary

amine, such as MEA or DEA, to the circulating prewash. Feeds with much higher levels
of acid gas require amine treating upstream of the prewash. Please refer to the Amine
Treating GOM if your unit has been designed with a UOP Amine Absorber.
6. Extraction Section
The mercaptan rich feed, free of H2S, CO2 and COS then enters the extraction section
of the Extractor PlusTM column where the feed is counter currently contacted with
caustic solution in a trayed tower. The circulating caustic solution contains dispersed
Merox catalyst, but the catalyst has no effect on mercaptan extraction. The
concentration of caustic in this section is typically 20° Be’.
During mixing, mercaptans transfer from the hydrocarbon feed to the caustic solution.
In a perfect or theoretical stage of contact, dynamic equilibrium would be reached. At
conditions of dynamic equilibrium, there is no further net transfer of mercaptans from
the hydrocarbon to the caustic; that is, the rate of mercaptan transfer from the
hydrocarbon to the caustic equals the rate of mercaptan transfer from the caustic back
into the hydrocarbon. In any real or actual stage of contact, true or complete
equilibrium is not reached. The closer the approach to true equilibrium, the more
efficient is the stage of contact.
The concept of the counter current principle is that as the gas proceeds upward tray
by tray, it is in contact with leaner and leaner caustic. Therefore, at the last stage of
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contact, the “cleanest” hydrocarbon is in contact with the leanest caustic. Conversely,
at the first stage of contact, the “dirtiest” hydrocarbon is in contact with the richest
caustic. This type of arrangement results in an approach to equilibrium favorable to
the least possible amount of mercaptan in the hydrocarbon leaving the top of the
extractor.
The trays specified are high efficiency jet decks, which permit the use of low caustic
rates. Because the caustic rates are low, the physical size of the caustic regeneration
section is relatively small. The extractor is simply a liquid-liquid countercurrent
contactor. Untreated hydrocarbon enters near the bottom tray of the contactor, and
regenerated caustic is pumped onto the top tray. Due to their gravity differences,
hydrocarbon will flow upward through the holes on the tray, while caustic will flow
across the trays and downward through the downcomers. The contactor is designed
so that intimate contact between the two liquids occurs. This is necessary to ensure
maximum mercaptan transfer from the hydrocarbon into the caustic.
5.3.2 CONTROL PHILOSOPHY
The arrangement of level controls is such that hydrocarbon flow surges across the
column are absorbed by the caustic hold up on the trays and at the bottom of the
column It is advisable to hold such a level in the Extractor during normal operation so
that maximum caustic surge space is available, consistent with surges in hydrocarbon
flow normally encountered. The Extractor is the only part of the plant that can be
seriously affected by surges in hydrocarbon flow. There is usually no problem with
surging flow on units charged with a pump. In many cases the unit will be charged
directly from a fractionating column in which case fluctuations in fractionator
instrumental control can cause surges in the Merox unit extractor. Fractionator controls
should be adjusted to give smooth control, by limiting flow rate changes to 10 vol% of
the feed rate over 1 hour.
Pressure within the Merox unit is controlled at two locations. The pressure of the
hydrocarbon section is maintained using a back pressure controller located after the
Post Treatment section, on the treated product line. The pressure is set high enough
to prevent hydrocarbon vaporization and create pressure drop needed for caustic flow
to the regeneration section. The pressure in the regeneration section is set to allow
disposal of the spent air stream and usage of plant air.
The caustic used in the extraction section will become diluted over time due to the
water produced during caustic regeneration. To maintain the circulating caustic
strength some of the circulating caustic needs to be removed and replaced with fresh
make up caustic.
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In the Continuous Caustic Prewash design caustic is transferred from the regeneration
section to the prewash section to maintain caustic concentration and achieve a better
overall caustic utilization. Regeneration caustic is added to the prewash section using
a timed flow controller valve located on the caustic transfer line from the caustic
circulation pumps. After caustic is transferred, if required it may be diluted to the
desired concentration by injecting water into the system.
In the case of an Enhanced Prewash, the caustic transferred from the regeneration
section must be accounted for when determining the required COS solvent
composition in the COS Solvent tank. When regenerated caustic is transferred from
the regeneration section fresh COS solvent is injected from the COS Solvent tank by
a timer to maintain the composition of the COS Solvent in the Prewash.
A level controller, located on the Prewash, is used to control aqueous solution being
removed from the Prewash through a control valve. As caustic transfers from the
regeneration section and COS solvent is added on a timed basis (if required), the
Prewash level rises and opens a control valve to send spent aqueous solution to the
Spent Caustic Degassing Drum and lowering the prewash level. The spent aqueous
solution is first degassed and then sent to safe disposal systems on gap control from
the Spent Caustic Degassing Drum. Fresh caustic must be added to the regeneration
section to make up caustic levels in the extraction section
Rich caustic flows from the Extractor to the regeneration section on level control from
the stack of the Disulfide Separator or on level control set point if there are more than
one Extractor sharing one regeneration section. Typically the smaller diameter will be
on level control set point at the bottom of the Extractor while the larger diameter will
be controlled by the stack of the Disulfide Separator.
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5.4 TROUBLESHOOTING
Troubleshooting of any process, should be an ongoing part of normal operations. Daily

records of operations are collected and should be reviewed to observe 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. This section is
focused on process related problems such as poor product quality or contamination
and operating problems for unique equipment. Troubleshooting of general equipment
such as pumps, compressors, and heat exchangers is not included since this
information is generally available from the equipment vendors.
5.4.1 EXTRACTION
Extraction efficiency may be affected by the following:
1) Insufficient caustic flow rate – indicated by excessive product mercaptan.

2) Excessive caustic flow rate – indicated by excessive product disulfide.
3) Excessive caustic neutralization or dilution (see Section VIII Normal
Operations).
4) Low hydrocarbon flow rate (relative to design flow rate).
5) Insufficient mercaptan solubility (higher boiling feedstock).
6) Excessive hydrocarbon feed temperature (reduced extraction efficiency).
7) Accumulation of non-regenerable acidic materials. In time, regardless of the
care used in prewashing, there will be some spending of the caustic due to
carbon dioxide present in the air injected into the Oxidizer. This is not typically
an issue, unless extremely high air rates are used. The more likely source of
non- regenerable acidic materials in a unit with a well run prewash is from the
wash oil used in the regeneration section.
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5.5.1 SAND FILTER BACKWASHING
As contaminants or impurities collect in the sand bed, it will lose its coalescing
efficiency and the differential pressure across the sand filter will gradually increase.
Initially the differential pressure across the filter will be negligible (near indiscernible).
When a differential pressure is apparent, as indicated by a difference of >14 kPa (>2
psi), the sand filter should be taken out of service for backwashing. Failure to do so
will result in continued differential pressure buildup and will lead to mechanical failure
of the sand support screen and inefficient coalescing of hydrocarbon impurities.
Backwashing should be conducted as follows:
a. Open the hydrocarbon line bypassing flow around the sand filter vessel and
block in the Sand Filter, including the equalization lines.
b. Pump out or drain the remaining hydrocarbon from the vessel. Displace the
hydrocarbon with steam or inert gas while taking the necessary precautions to
ensure that the vessel is maintained under a slight positive pressure at all times.
In the case of LPG, depressure the sand filter to the flare and displace the
residual vapors with water.
c. Open the backwash line provided at the sand filter inlet line, removing the blind,
if provided.
d. Connect a temporary water supply to the connection provided at the vessel
drain.
e. Begin filling with water.
f. When the vessel is full of water, flush at a vigorous water flow rate, upflow
taking care that no sand is floated out the inlet.
g. The backwashing may be considered complete when the effluent is essentially
clear and free of suspended matter.
h. Put Sand Filter back into service, using safe refinery practices.
5.5.2 LEAK TEST INSTRUCTIONS
These instructions are for leak testing the inlet and outlet weirs (downcomers included)
on the Merox Extractor and Amine Absorber columns. It is recommended that the leak
testing be conducted initially on the lowest tray and then on each subsequent upper
tray. All tray manways need to be removed for the leak test.
a. Check the level on the weir top edge. The edge should be level. Repair or
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adjust the level as necessary as per the specified tolerance.

b. Tightly plug the downcomer with the blind plate and neoprene gasketing.
c. Plug the inlet weir weep hole if one exists with a plug, cloth, plastic or other
suitable material.
d. Starting with the bottom trays, carefully fill the inlet and outlet weirs to
approximately ¼” from the top of the weir plate with water. This can most
conveniently be done with a long hose with an on/off valve on the end. Try to
minimize the spillage outside of the weir pans to avoid the amount of drying
required.
e. Very thoroughly dry all areas of the tray and vessel shell underneath the outlet
and inlet weir pans using cloths or an air hose. This will allow any leaks present
to be very easily identified.
f. Check all weld points:
i.) On the downcomer,

ii.) Where the downcomer connects with the outlet weir bottom pan,
iii.) Along all edges of the inlet and outlet weirs, both above and below the
tray (weir sides, weir pan bottom, edges immediately above and below
the tray.
iv.) Note that no leaks, dripping, or seeping is allowed! Mark any of these
defects for repair with a crayon or chalk.
g. Unplug the downcomer and the weir weep hole to drain all the water.
h. Repair any and all leaks found as marked per UOP recommendations. Repeat
from Step 4 upon the completion of the repairs until no leaks, dripping, seeping
or sweating are evident.
i. Remove the downcomer blind plates.
j. Ensure that the trays are clean of all debris and/or dirt before proceeding with
closing of the tray manways. (Note: When installing the tray manways, verify
that the tray manways are correctly installed so as the specified equilateral
pitch is maintained across the manway and tray.) A one-piece neoprene gasket
should be used for the tray manways.
5.5.3 BATCH PREWASH CAUSTIC CHANGE OUT

INSTRODUCTIONS USING FRESH CAUSTIC
Before beginning caustic preparations, confirm that the condensate or demineralized

water and caustic are below 60°C (140°F) and that the steam tracing on these lines
are on only if necessary to prevent freezing. Caustic embrittlement begins at 65°C
(150°F) for non-PWHT carbon steel. Higher temperatures may also cause small
amounts of the LPG to flash when it contacts the hotter aqueous phase, causing
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operational upsets..
a. Take a sample of the caustic in the Caustic Prewash Vessel via the Sample
Station. If the caustic is between 50-70% spent or if H2S breakthrough is
occurring, then a caustic change out is necessary.
b. Verify that the globe valve on the caustic filling line is closed. The gate and
globe valves on this line to the Extractor should also be closed.
c. Verify that the gate and globe valves on the caustic transfer line are closed.
d. Confirm that the Spent Caustic Degassing Drum level glass and level
transmitter are ready for servicing.
e. Prepare to operate one of the Spent Caustic Pumps by opening the isolation
valves to one of the pumps. Verify that the automatic on/off switch is ready for
servicing. This switch should turn the pump on at a high level (i.e. 80%) in the
Spent Caustic Degassing Drum and should turn the pump off at a low level (i.e.
20%).
f. Make sure the Spent Caustic Disposal System is ready to receive caustic.
g. Slowly open the gate valve to the top inlet distributor and close the bottom,
gate valve on the bottom distributor. This switches the direction of the flow to
minimize entrained LPG exiting with the caustic.
h. Open the drain gate valve at the bottom of the Caustic Prewash.
i. Begin to send caustic to the Spent Caustic Degassing Drum by slowly opening
the gate and globe valves on the waste transfer line. Control the flow by taking
½ of the pressure drop across the globe valve and the rest across the
restriction orifice.
j. Watch the level in the Caustic Prewash carefully. When the Caustic Prewash
level has decreased to approximately 10% 30%, or 300 mm (1 foot) above
the inlet distributor, close the gate and globe valves on the waste caustic
transfer line. Do not drain the level below the inlet distributor to avoid losing
the contact between hydrocarbons and caustic, which would result in H2S carry
over to the Extractor, especially when very high levels of H2S are present in
the feed.
k. Prepare to add caustic to the Caustic Prewash vessel by opening the gate
valve on the caustic inlet line. Make sure the Water Break Tank is isolated at
the outlet before opening this valve!
a. If using the regeneration caustic for batch change out of the prewash, skip
to letter “a” of the next section titled
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5.5.4 PREWASH CAUSTIC CHANGEOUT INSTRUCTIONS

USING REGENERATED CAUSTIC
a. Open the globe valve on the caustic filling line to the Caustic Prewash.
b. Start the Water/Caustic Addition Pump (if provided) and begin transferring
caustic to the Caustic Prewash Vessel. Fill caustic to 50%. Watch this addition
carefully to avoid filling the Caustic Prewash too quickly and/or too high and
risk causing caustic to carry over into the Extractor.
c. Ultimately, the total aqueous solution height in the Caustic Prewash should be
at 50%. However, if the caustic supply concentration is greater than 12wt%
(17° Bé), caustic should be added to below 50% to allow for the volume of
water which will be added to reduce the combined caustic strength in the
Caustic Prewash to 5-10 wt% (8-15° Bé). If the fresh caustic concentration is
within 5-10 wt%, additional water will not be necessary and the caustic can be
added to 50%.
d. When the level is 50% of the Caustic Prewash vessel, stop the Water/Caustic
Addition Pump and close the gate valve on the caustic inlet line.
e. Add MEA to ratio of MEA to NaOH needed for COS removal
f. If the caustic supply concentration is greater than 10 wt% (15° Bé), water will
have to be added to dilute the caustic. Prepare to add water to the Caustic
Prewash by lining up the water to the Water/Caustic Addition Pump.
g. Start the Water/Caustic Addition Pump and begin transferring water to the
Caustic Prewash Vessel. Add water up to 50%. (This level should be marked
on the level glass.) Watch this addition carefully, so as not to add too much
water and dilute the caustic or risk having caustic carryover into the Extractor
due to a high caustic level.
h. When the level is at 50%, stop the Water/Caustic Addition Pump and close the
gate valve on the outlet line from the Water Break Tank.
i. Close the globe valve on the caustic filling line.
j. Close the filling/draining gate valve at the bottom of the Caustic Prewash.
k. Slowly open the gate valve on the lower inlet distributor. Close the gate valve
on the upper inlet distributor.
l. The LPG flow through the inlet distributor will help to further mix the caustic
solution. Wait 2 hours and sample the prewash caustic for total alkalinity. The
target caustic concentration is 5-10 wt% (8-15° Bé). If the total alkalinity is
greater than 10 wt%, add more water. If more water is needed, it will be
necessary to drain some of the prewash caustic before adding more to avoid
overfilling. Do not operate the Caustic Prewash vessel with a level greater than
50% to avoid the risk of having caustic carryover into the Extractor.
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5.5.5 ENHANCES PREWASH BATCH COS

SOLVENT CHANGE OUT
Before beginning, confirm that makeup COS Solvent is available in the COS Solvent
tank. Sample the COS Solvent to confirm the composition meets the desired
specification.
NOTE: Typically the COS Solvent Tank composition will take in to account the daily
transfer of regenerated caused from the Regeneration section to the Prewash. This
means that the COS Solvent tank composition will contain less caustic than is required
to treat the feed. This lack of caustic can be rectified by adding fresh caustic directly
to the Prewash, this avoids having to adjust the composition of the entire COS Solvent
Tank and allows normal operation to continue after the change out.
The COS solvent temperature should be below 60°C (140°F), note that the steam
tracing on these lines should only be turned on only if necessary to prevent freezing.
Caustic embrittlement begins at 65°C (150°F) for non-PWHT carbon steel. Higher
temperatures may also cause small amounts of the LPG to flash when it contacts the
hotter aqueous phase, causing operational upsets.
a. If there is an upset and H2S/COS breakthrough is occurring, then a batch

change out of the COS Solvent might be necessary to quickly get the unit back
on specification.
b. Sample the circulating COS solvent to confirm if it has become spent and a
change out is required. Typically COS solvent should be changed out when
the apparent MEA content of the solution has fallen below 2 wt%.
c. Verify that the globe valve on the COS Solvent filling line is closed.
d. Confirm that the Spent Caustic Degassing Drum level glass and level
transmitter are ready for service.
e. Prepare to operate one of the Spent Caustic Pumps by opening the isolation
valves to one of the pumps. Verify that the automatic on/off switch is ready for
servicing. This switch should turn the pump on at a high level (i.e. 80%) in the
Spent Caustic Degassing Drum and should turn the pump off at a low level (i.e.
20%).
f. Make sure the Spent Caustic Disposal System is ready to receive spent COS
solvent.
g. Begin to send spent COS solvent to the Spent Caustic Degassing Drum by
slowly opening the gate and globe valves on the waste transfer line. Control
the flow by taking ½ of the pressure drop across the globe valve and the rest
across the restriction orifice.
h. Watch the level in the Prewash carefully. When the Prewash level has
decreased to approximately 10%, close the gate and globe valves on the waste
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caustic transfer line. Do not drain the level below the inlet distributor to avoid
losing the contact between hydrocarbons and caustic, which would result
in insufficient COS removal and H2S carry over to the Extractor, especially
when very high levels of H2S are present in the feed.
i. Prepare to add COS solvent to the Enhanced Prewash by opening the gate
valve on the COS solvent filling line.
j. Open the globe valve on the COS solvent filling line to the Prewash.
k. Start the COS Solvent Addition Pump and begin transferring COS Solvent to
the Prewash Vessel. Fill COS Solvent to 50%. Watch this addition carefully to
avoid filling the Prewash too quickly and/or too high and risk causing carry over
into the Extractor.
l. Ultimately, the total aqueous solution height in the Prewash should be at 50%.
However, if additional caustic will be supplied from the regeneration section,
COS solvent should be added to below 50% to allow for the volume of caustic
which will be added to adjust the COS solvent composition.
m. When the level is 50% of the Prewash vessel, stop the COS Solvent Addition
Pump and close the gate valve on the caustic inlet line.
n. Close the globe valve on the COS solvent filling line.
o. Close the filling/draining gate valve at the bottom of the Prewash.
Allow the solution to circulate for a while and then sample the circulating COS Solvent
to check the composition meets the required specification. If the composition is not
correct then it might be necessary to adjust by either adding more fresh COS solvent
or more caustic, in this case it may be necessary to drain some more spent solvent
from the prewash first. Do not operate the Caustic Prewash vessel with a level greater
than 50% to avoid the risk of having caustic carryover into the Extractor.
5.5.6 PREWASH CAUSTIC CHANGE OUT

INSTRUCTIONS USING REGENERATED CAUSTIC
In order to utilize the caustic in the unit to its fullest extent, the regenerated caustic,
which is typically less than 10% spent, can be transferred and used in the Caustic
Prewash when change out of the prewash caustic is necessary. This prewash caustic
can then be further used until the caustic is 50% spent (70% maximum). Note that the
prewash caustic should not be changed out until the percent spent is 50-70%. If other
considerations require that the regeneration caustic be changed out, remove only
enough caustic from the Caustic Prewash to accommodate the quantity of caustic that
will be removed from the Extractor and regeneration section, without having to add
fresh caustic to the Caustic Prewash. This will minimize the overall caustic
consumption. While similar to the Prewash Caustic Change out Instructions Using
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Fresh Caustic, deviations do exist that should be noted. These include
• Dilution of the caustic prewash when required by the schedule A due to the
higher regeneration caustic concentration,
• Preparation and careful monitoring of the regeneration section during the

transfer,
• Addition of fresh caustic to the regeneration section to make-up caustic loss to

the prewash
• Addition of Merox WS-2 catalyst to maintain catalyst concentration diluted by

addition of fresh caustic to the circulating caustic. The procedures that follow
outline this method.
Please note: Due to the sulfidic nature of the prewash caustic, the prewash
caustic cannot be used in the regeneration section.
Before beginning caustic preparations, confirm that the condensate or demineralized

water and caustic are below 60°C (140°F) and that the steam tracing on these lines
are on only if necessary to prevent freezing. Caustic embrittlement begins at
approximately 65°C (150°F) for non-PWHT carbon steel. Higher temperatures may
also cause small amounts of the LPG to flash when it contacts the hotter aqueous
phase, causing operational upsets.
a. Remove caustic using steps a – j in the previous section D – PREWASH

CAUSTIC CHANGEOUT INSTRUCTIONS USING REGENERATED
CAUSTIC,
b. Open the gate valve on the caustic transfer line to the Caustic Prewash.
c. Prepare to transfer lean caustic from the Caustic Circulation Pumps by opening
the gate valve on the caustic transfer line from the Circulation Pumps.
d. Slowly open the globe valve on the caustic transfer line and slowly begin
transferring lean caustic from the Regeneration Section to the Caustic
Prewash. NOTE: To avoid decreasing the lean caustic flow to the top of the
Extractor, it may be necessary to either start the spare Caustic Circulation
Pump or to close the minimum flow spillback, if present. The extractor level
should be watched very carefully during this step! When the Extractor level
reaches 20%, caustic transfer to the Caustic Prewash should be stopped and
the globe valve on the caustic transfer line from the Caustic Circulation Pumps
closed. Also close the gate valve on the caustic transfer line. (Confirm that a
level of 20% will not interfere with the Low Level Shut Off Valve on the Extractor
outlet line.) The interface level in the Disulfide Separator should not be
reduced during this step!
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e. While transferring caustic from the Regeneration Section into the Caustic
Prewash, the Caustic Prewash level should also be monitored. Caustic should
be filled to below 50% of the height of the Caustic Prewash vessel, however
the Extractor level will more likely reach 20% before the Caustic Prewash level
reaches below 50%. Watch the caustic transfer carefully to avoid filling the
Caustic Prewash too quickly and/or too high and risk causing caustic to
carryover into the Extractor.
f. Ultimately, the total aqueous solution height in the Caustic Prewash should be
at 50%. However, caustic should be added to below 50% to allow for the
volume of water which will be added to reduce the combined caustic strength
in the Caustic Prewash to 5-10 wt% (8-15° Bé).
g. If this is an Enhanced Prewash, add MEA to ratio of MEA to NaOH needed for
COS removal
h. If the Extractor level reaches 20% before the Caustic Prewash level reaches
50%, as expected, fresh caustic will need to be added to the regeneration
section as make up.
i. Since the regeneration caustic and fresh caustic supply concentrations are
usually greater than 10 wt% (15° Bé), add water to dilute the caustic. Prepare
to add water to the Caustic Prewash by lining up the water to the Water/Caustic
Addition Pump.
j. Start the Water/Caustic Addition Pump and begin transferring water to the
Caustic Prewash Vessel. Add water up to 50%. (This level should be marked
on the level glass.) Watch this addition carefully, so as not to add too much
water and dilute the caustic or risk having caustic carryover into the Extractor
due to a high caustic level.
k. When the level is at 50%, stop the Water/Caustic Addition Pump and close the
gate valve on the outlet line from the Water Break Tank.
l. Close the globe valve on the caustic filling line.
m. Close the filling/draining gate valve at the bottom of the Caustic Prewash.
n. Slowly open the gate valve on the lower inlet distributor. Close the gate valve
on the upper inlet distributor.
The LPG flow through the inlet distributor will help to further mix the caustic solution.
Wait 2 hours and sample the prewash caustic for total alkalinity. The target caustic
concentration is 5-10 wt% (8-15° Bé). If the total alkalinity is greater than 10 wt%, add
more water. If more water is needed, it will be necessary to drain some of the prewash
caustic before adding more to avoid overfilling. Do not operate the Caustic Prewash
vessel with a level greater than 50% to avoid the risk of having caustic carryover into
the Extractor.
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5.5.7 EXTRACTOR LEVEL REPLENISHMENT WITH FRESH

CAUSTIC:
a. Open the gate valve completely and crack open the globe valve on the caustic
filling line to the Extractor.
b. Prepare to add fresh caustic to the Extractor by opening the gate valve on the
fresh caustic inlet line. Make sure the Water Break Tank is isolated at the outlet
before opening this valve!
c. Start the Water/Caustic Addition Pump (if provided) and slowly begin
transferring fresh caustic to the Extractor. Fill caustic to 50% of the surge
volume, as seen on the level glass. Watch this addition carefully to avoid
filling the Extractor too quickly and/or with too large a volume and risk causing
caustic to carryover. The addition rate can be controlled using the globe valve
on the caustic transfer line.
Note: If the addition rate is more than 10 vol% of the hydrocarbon rate,
the tray seal may be broken and massive caustic carryover will occur.
d. Depending on the strength of the regeneration caustic, the strength of the fresh
caustic supply and the quantity of caustic added, water may have to be added
to dilute the regeneration caustic. (Note that if water will have to be added, the
caustic should be filled accordingly so the final extractor level is between 40 -
60%.) Prepare to add water to the Extractor by lining up the water to the
Water/Caustic Addition Pump.
e. Open the gate and globe valves on the caustic filling line at the Extractor.
f. Start the Water/Caustic Addition Pump and begin transferring water to the
Extractor. Add water up to target 50% of the surge volume. (This level should
be marked on the level glass.) Watch this addition carefully, so as not to add
too much water too quickly and dilute the caustic or risk having caustic
carryover.
g. When the level is at 50% of the Extractor surge volume, stop the Water/Caustic
Addition Pump and close the gate valve on the outlet line from the Water Break
Tank.
h. Close the globe and gate valves on the caustic filling line at the Extractor.
i. Finally, Merox Reagent WS-2 catalyst should be added to the system to
compensate for the estimated fresh caustic/water addition. Add additional
catalyst to about 1 gallon for every 1000 gallons (4 m3) of caustic added)
The ideal, targeted Extractor level is 50%. This will slowly increase to 80% over time,
as mercaptan in the feed will form water upon contact with the caustic and will dilute
the regeneration caustic, increasing the Extractor level. Further, this Extractor surge
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level will drastically change with large hydrocarbon flowrate changes. Based on
experience, refiners should determine the optimum Extractor level that best
accommodates the dilution effect of the particular unit and the stability (or instability)
of the hydrocarbon flowrate.
5.5.8 SAND FILTER LOADING INSTRUCTIONS
Prior to starting the loading the Sand Filter, confirm that a sufficient amount of 8-16
mesh quartz silica sand is available for loading.
a. Verify that the vessel is completely blinded and isolated.

b. Verify that the line leading to and from the level glass are closed.
c. After the Sand Filter is mechanically complete, open the top manway.
d. Verify that the Sand Filter is clean inside and that no garbage is on the grid.
e. Tightly cover the distributor slot with a plastic tarp or other suitable material to
prevent sand from entering the distributor.
f. Begin adding sand from the side manway. Add enough sand to cover the
support by 2 to 4 inches. Confirm that the sand has not leaked through.
g. Once the support has been determined to be stable, perform a final closure on
the side manway and continue loading sand from the top manway. Level the
sand once the sand nears the top and measure the distance from the middle
of the distributor to the top of the bed.
h. Fill the sand until the level top of the bed is 450 mm (18") below the center of
the distributor, or as specified in the vessel drawing of the Schedule A. Make
sure the bed is leveled well.
i. When the loading is completed, uncover the distributor and close the top
manway with the proper gasket installed.
j. Note the quantity of sand loaded for future reference and complete the loading
diagram.
5.5.9 SAND FILTER UNLOADING PRECAUTIONS
When a reduction in the pressure drop across the sand filter cannot be achieved via a
backwash, or when the frequency of backwashing becomes impractical, then the sand
in the Sand Filter will have to be replaced. Prior to removing the sand from the vessel,
safety considerations recommend that a backwash be performed to remove any
caustic and/or residual hydrocarbon from the sand before handling. After sufficiently
backwashing the sand, the side and top manways can be opened for manual and/or
vacuum removal of the sand.
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6. CAUSTIC MEROX COVENTIONAL

REGENERATION
6.1 INTRODUCTION
6.1.1 MEROX PROCESS OVERVIEW

The UOP Merox Process is an efficient and economical catalytic process developed
for the chemical treatment of petroleum distillates for removal of sulfur present as
mercaptans (Merox Extraction) or conversion of mercaptan sulfur to a less
objectionable form (Merox Sweetening). The process relies on UOP developed
catalyst, specifically designed to accelerate the oxidation of mercaptans to disulfides
at economical product rundown temperature.
The Merox process is based on the ability of a catalyst composed of iron group metal
chelates to promote the selective oxidation of mercaptans to disulfides in an alkaline
environment, using air as the source of oxygen. This technique has long been known
but was generally impractical without a catalyst. It was not until UOP introduced Merox
catalyst in 1958 that the great economic advantage of regeneration of caustic by use
of atmospheric oxygen was fully realized (see Figure I-1).
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Figure I-1
Oxidation of Mercaptans with Air and Caustic
The reaction proceeds at an economically practical rate at normal temperatures for

refinery rundown streams. For liquid stocks, operating pressure is controlled above
the bubble point to assure liquid phase operation. Downstream pressure requirements
are easily taken care of by use of appropriate size product pumps.
Merox treatment can, in general, be utilized in the following ways:
1) Odor improvement on all stocks.

2) Reduce sulfur content of products to meet specifications for motor fuel or other
combustion processes.
3) Reduce sulfur content of FCC, coker or visbreaker C3/C4 olefins resulting in
decreased acid consumption during alkylation operations using these
materials as feedstocks.
4) Meeting the requirement of low sulfur for sensitive catalyst used in various
chemical synthesis processes.
6.1.2 MEROX ADVANTAGES
Relative to other treating processes, the Merox Process has the following advantages:
1) Low operating cost and investment requirement. The initial investment in many
applications can be very low based on the conversion of existing equipment
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for use in Merox Treating processes and minimal plot area requirement. Low
utility and chemical usage result in low operating costs.
2) Ease of operation. Merox Process Units are simple to operate; the air injection
rate is the only direct adjustment necessary to accommodate wide variations
in feed rate or mercaptan content. Operating labor requirements are minimal.
3) Proven reliability. The Merox process has been widely accepted by the
petroleum industry; over 1800 units of various kinds (extraction, liquid, and
fixed bed sweetening) have been placed in operation.
4) Minimal chemical disposal requirements.
Proven ability to produce on specification products. There is no product deterioration

due to side reactions or need for addition of undesirable materials to the treated
product.
6.1.3 HISTORY OF THE UOP MEROX PROCESS
The 1500th UOP Merox Unit started initial operations on October 19, 1993, currently
there are over 1800 units in operation across the world.
The remarkable popularity of the UOP Merox process around the world is unrivaled by
any other petroleum refining process and very few oil refineries are in operation
without one or more Merox Units to treat the products. The popularity of the UOP
Merox Process can be attributed to its economical operation, ease of control, and
ability to chemically treat mercaptans in a manner unique to Merox.
The basic Merox patents were issued to UOP researchers W. K. T. Gleim, et al. in the
late 1950's and early 1960's. The manager of the UOP Treating Department, Kenneth
M. Brown, saw the myriad advantages for the Merox catalyzed mercaptan oxidation
over the other available processes and set out to convince UOP management to
commercialize the process. At this point in time, the major treating processes in
commercial use were:
Caustic Extraction/Steam Regeneration – for gas streams, LPG and light gasoline
Caustic Scrubbing/Inhibitor Sweetening – for FCC and light thermal gasoline
Copper Chloride Sweetening – for low mercaptan feedstocks
Doctor Sweetening – for high mercaptan feedstocks
Having spent 20 years trying to develop procedures to understand and overcome the
shortcomings of these processes, Ken Brown is credited with developing and molding
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the research work into a viable, economical, commercial refinery process which we
today call "Merox".
During the 1960's, UOP continued to improve the Merox process and its application to
the treatment of LPG (extraction), FCC and light gasolines (liquid-liquid sweetening),
and kerosene and jet fuels (fixed bed sweetening). In the early 1970's, changes in
FCC Unit operations led to the development of the Minalk version of the fixed bed
sweetening process. The first extraction unit treating a mercaptan rich gaseous
methane stream was put in service in 1976. In the same year, two, relatively new,
easy-to-use Merox catalyst were commercialized and an entirely new catalyst for
sweetening kerosene feed stocks was created.
In 2001, customers were given the option of using the Extractor Plus™ design. The
new design combines the functions of the Caustic Prewash, Extractor, Caustic
Knockout Drum and Sand Filter vessels into one column. The use of a multifunctional
column reduces unit plot area and results in a reduction of the initial investment cost
for the unit. Other features of the new design are: continuous caustic prewash
circulation, caustic heater and oxidizer outlet temperature control, continuous Merox
catalyst injection, and improved handling of the spent gas stream.
In 2010 UOP released the design of the Disulfide Scrubber. The new lean caustic
wash oil system greatly reduces the disulfide content in the lean caustic. The packed
bed column achieves this by counter current contact of the lean caustic against the
wash oil phase. Application of this technology allows ultra-low product sulfur
concentrations of less than 1 wppm to be achieved.
In 2013 UOP introduced the Enhanced Prewash Section for H2S, CO2 and COS
Removal, located at the bottom of the Extractor Plus column. The hydrocarbon
feedstock enters the bottom section of the prewash after being contacted with a
circulating aqueous mono- or di-ethanolamine [MEA or DEA] and NaOH solution for
COS removal. The COS present first reacts with the MEA to release H2S which is then
quickly absorbed by the sodium hydroxide. Any H2S present in the hydrocarbon will
also be removed in this section.
In 2014 UOP released the MVP Regeneration design: This Modular Equipment
offering optimizes the design of the traditional Merox caustic regeneration section
redesigning to reduce the size and number vessels required. This results in plot space
reduction of more than 25% when compared to the conventional regeneration design.
Upgraded technology of the MVP Regeneration includes all the benefits of the disulfide
scrubber for ultra-low product sulfur while simplifying operation and improving safety
by reducing the volume of spent air by 25% and sulfur emissions by more than 90%.
Over the years, the UOP Merox process has revolutionized the refining industry in the
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chemical treatment of petroleum products. It is UOP's constant aim to improve and

simplify the Merox process and to educate our licensees in its application. There was
a time when treating was an art, not a science, practiced in the far corners of the
refineries by people long suspected of possessing magical rather than technical skills.
Today there exists a sound logical understanding of chemical treating which needs
only to be put into practice.
The distribution of operating Merox Units by type is approximately:
Extraction 32%
Extraction + Sweetening 12%
Minalk Fixed Bed Sweetening 14%
Kerosene and Jet Fuel Sweetening 42%
Table I-1 illustrates the applications for treating the various streams via the Merox
process.
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Table I-1
Applications of the Merox Process
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6.1.4 GENERAL TREATING TERMS

Azeotrope a mixture of substances that behaves as a single substance in
that the vapor produced by partial evaporation has the same
composition as the liquid.
Antioxidant chemical additive to inhibit oxidation reaction
Barrel 42 U.S. gallons measured at 60°F
BPD barrels per day (also BSD)
Caustic sodium hydroxide solution
C/H caustic/hydrocarbon volume ratio
delta P (dP) differential pressure
delta T (dT) differential temperature
disulfide class of sulfur compounds characterized by a sulfur-to-sulfur

bond and relatively low volatility represented by the general
formula RSSR
EP endpoint (ASTM distillation)
Enhanced Current design configuration that removes H2S, CO2, and COS
Prewash from the hydrocarbon prior to extracting the mercaptans
Extraction removal of mercaptan sulfur from hydrocarbon
Extractor Plus™ current design configuration of the extraction version of the Merox
process. A caustic prewash section for H2S removal, a mercaptan
extraction section, and a coalescing section to remove entrained
caustic are integrated into one column.
GC or GLC gas chromatography
Gph U.S. gallons per hour
Gpm U.S. gallons per minute
Gum polymerized hydrocarbon

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hydroperoxide compound responsible for propagation of gum forming chain

reaction (-OOH)
IBP initial boiling point (ASTM distillation)
Inhibitor compounds responsible for delaying or terminating a chemical

reaction
LHSV liquid hourly space velocity
mercaptan common name given to class of compounds having thiol

functional groups represented by the general formula RSH
Merox® Process a UOP licensed process that uses a metal based catalyst to
oxidize mercaptan sulfur to disulfide oil
MVP Current regeneration design configuration that accomplishes all

of the regeneration section operations in 2 vertical vessels,
minimizing vessels and plot space
naphthenic acid organic (carboxylic) acid
Nm3 normal cubic meter (1 atm. 0°C)
std. m3 standard cubic meter (1 atm. 15°C)
organo-metallic complex compound characterized by weak carbon to metal

bonds
ppm parts per million
PW prewash
re-entry sulfur entrained disulfide sulfur in regenerated caustic that enters and
dissolves into the exiting hydrocarbon product from an extractor
RX reactor
SCFH standard cubic feet per hour (1 atm. 60°F)
sweetening conversion of mercaptan to disulfide without desulfurization
Stability quality of a fuel to remain unchanged for long periods of time in

storage
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Thiol sulfur-to-hydrogen bond
thiophenol common name given to aryl mercaptans; also the compound

C6H5SH
vol., vol% volume, volume percent
vppm volume (mole) parts per million
wt., wt% weight, weight percent
wppm weight parts per million

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6.1.5 CHEMICAL ABBREVIATIONS AND SYMBOLS

A• inhibitor free radical
C carbon
C1 hydrocarbon with 1 carbon atom (e.g., methane)
C2 hydrocarbon with 2 carbon atoms (e.g., ethane)
Cn hydrocarbon with n carbon atoms
CaCO3 calcium carbonate
CO2 carbon dioxide
H hydrogen
H2S hydrogen sulfide
Na sodium
NaHS sodium bisulfide
Na2CO3 sodium carbonate
NaOH sodium hydroxide (caustic)
Na2S sodium sulfide
NaSR sodium mercaptide
Na2S2O3 sodium thiosulfate
O oxygen
O2 diatomic oxygen (normal form in gaseous state)
R- alkyl group side chain
R• alkyl free radical
RSH mercaptan
RSSR disulfide
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S sulfur
S° elemental sulfur
-SH thiol (mercapto functional group)
unsaturated cyclic hydrocarbon compound
saturated cyclic hydrocarbon compound
[] solution concentration (moles/liter)

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This section discusses the major Merox process variables and their effect on
performance. Specific emphasis will be placed on identifying the optimum operating
conditions. The following represent the five primary process variables. Each will be
discussed as an independent with all others held constant.
C atalyst
O xygen
A lkalinity
C ontact
H eat
6.2.1 CATALYST CONCENTRATION
The extractive Merox process requires the use of UOP Merox Reagent WS-2. It is
supplied as a dark blue solution packaged in 2 U.S. gallon (7.6 liter) sealed
polyethylene bottles. Alternatively, Merox WS-2 can be supplied in 55 U.S.-gallon
drums and 330 U.S-gallon IBC containers.
Catalyst concentration is a direct operating variable in the extraction process. For initial
makeup, or whenever fresh caustic is added to replenish the system, a catalyst
concentration of approximately 0.1 Volume Percent in the caustic is recommended.
This corresponds to 1 gallon of Merox WS-2 per 1000 U.S. gallons of caustic inventory
loaded (1 liter per 1000 liters of caustic inventory loaded). A regular schedule of
catalyst addition must be followed to maintain this catalyst activity concentration. As
an initial recommendation, catalyst should be added at a rate of:
1 gallon per 22,000-50,000 barrels (1 liter per 920 to 2,100 cubic meters) of
hydrocarbon feed
Catalyst addition rate may be optimized accordingly as long as plant performance is

maintained.
Note: A formal, analytical method to determine active catalyst concentration in

the Merox caustic does not exist. However, the shake test result can determine
if more catalyst is needed.
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6.2.2 OXYGEN INJECTION
Oxygen is supplied to the caustic regeneration section of the Merox Unit in the form of
compressed atmospheric air. The stoichiometric, or theoretical, amount of oxygen
necessary is 0.25 kg per kg of mercaptan sulfur (or 0.25 pounds oxygen per pound of
mercaptan sulfur). At standard conditions of temperature and pressure, one cubic
meter of air, contains about 0.28 kg of oxygen (one cubic foot of air contains about
pounds of oxygen). Therefore, about 0.88 std m3 of air is needed for each kg of
mercaptan sulfur to be oxidized (14.2 SCF air per pound of mercaptan sulfur). It is
necessary to have at least a slight excess of oxygen present. The amount of excess
air injection is highly dependent upon the individual feedstock, but normally ranges
between 1.2 to 2.0 times the theoretical requirement. Thus, an initial injection rate at
2.0 times theoretical may be calculated from the formula below:
(Air) = 2.0 (K) (Feed rate) (S.G.) (RSH)/(10,000)
For liquid phase feed - where:
English Metric
Air = Air injection rate SCFH std m3/hr
K = Constant 2.07 8.81
Feed rate = Feed flow rate BSD m3/hr
S.G. = Specific gravity @ 60°F 15°C
RSH = Mercaptan sulfur wppm wppm
A graph of this formula, as shown in Figure III-1, is helpful in maintaining the proper
air injection rate as the feedrate and mercaptan level varies.
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Figure III-1
Air Injection Rate
(Air) = 2.0 (K) (Feed rate) (MW) (RSH)
For gas phase feed where:

English Metric
Air = Air injection rate SCFH std m3/hr
K = Constant 0.00155 0.00155
Feed Rate = Feed flow rate MMSCFD MM std m3/day
Fuel gas molecular weight lb/lb mole kg/kg mole
RSH = Mercaptan sulfur wppm wppm

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A graph of this formula, as shown in Figure III-2, is helpful in maintaining the proper
air injection rate as the feedrate and mercaptan level varies.
Figure III-2
Air Injection Rate
During operation of extraction Merox Units, the air is mixed with the rich caustic flowing
to the oxidation section. All other variables being equal, an increase in air injection
results in a more rapid and complete caustic regeneration. Thus, the regenerated
caustic returning to the extractor would contain relatively lower sodium mercaptide
concentration and possess a greater capacity to extract mercaptan. However,
increasing air injection decreases residence time in the oxidizer. Unless an unusually
large excess of air is used, this has little effect.
While a low mercaptan concentration is desirable, the caustic should never be

completely regenerated for the following reasons:
a) Oxygen can dissolve in the caustic and cause sweetening to occur in the
extractor.
b) The excess spent air will have a higher oxygen concentration that may result
in increased corrosion and potential hazards.
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Maintaining a small amount of mercaptide in the circulating caustic ensures better

catalyst solubility in the aqueous caustic
6.2.3 ALKALINITY
Alkalinity is provided by aqueous sodium hydroxide, or caustic, solution. Other

synonymous terms include caustic soda and lye. In this manual “caustic” is the generic
term used. Caustic is the solvent provided for mercaptan extraction and also the
medium in which the catalyst is dispersed. In addition, it provides the alkaline
environment necessary for the mercaptan oxidation reaction to proceed.
For mercaptan extraction, 20° Baume (14.4 wt-% or 4.15 g-mol/liter) caustic is the
optimum concentration for dissolution of the light mercaptans present. However it is
also optimum density to separate caustic from washoil and disulfide oil. Since disulfide
oil is close to the same density as water, more dense caustic solution will result in
quicker separation in the Disulfide Separator.
An upper limit of 25° Baume (19 wt%) is the maximum practical concentration. Above
this strength, viscosity and surface tension can promote emulsions and cause disulfide
oil to become difficult to separate and return to the Extractor in the lean caustic.
6.2.4 CONTACT
The Oxidizer has a specially designed distributor which promotes contact through
good mixing. The highly efficient distributor along with carbon raschig rings further
ensure gas/liquid mixing for mass transfer of oxygen from the gas phase to the
aqueous caustic phase. The more mass transfer of oxygen from air to caustic, the
faster the disulfide reaction.
The anthracite coal bed in the Disulfide Separator also uses contact to coalesce
disulfide and wash oil from the caustic phase. The tight size gradation, crushed and
screened to fall between the #4 and #8 ASTM mesh, of the anthracite coal, combined
with its nonpolar character and sharp edges collect, coalesce, and separate the
nonpolar wash oil and disulfide oil. Poor loading practices or retaining grid failure will
cause a channel to form and lead high product sulfur due to reentry sulfur.
Contact is also critical in the static mixer of a Two Stage Wash Oil system or the
packing of the Disulfide Scrubber. Correct pressure drop and wash oil rates ensure
good mass transfer of disulfide oil from the caustic to the wash oil phase. Any entrained
disulfide oil remaining in the regenerated caustic as it enters the top of the extractor is
completely extracted by the exiting hydrocarbon stream (see Figure III-5). Sulfur in the
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Merox product as a result of this effect is referred to as re-entry sulfur (Equation V-1).
At a constant feed rate, re-entry sulfur increases in the treated hydrocarbon in direct
proportion to the caustic circulation rate increase.
Figure III-3
Re-entry Sulfur
Since increasing the caustic to hydrocarbon ratio increases re-entry sulfur

proportionally and decreases mercaptan sulfur exponentially, there exists a single
optimum ratio where total mercaptan sulfur plus re-entry sulfur is minimized (see
Figure III-6). Above the optimum C/H ratio, increased re-entry sulfur can be excessive;
below it, mercaptan sulfur extraction may be inadequate.
Figure III-4
Optimum Castic
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6.2.5 HEAT (TEMPERATURE)
The Merox caustic regeneration reaction is favored by higher temperature. Thus, in

Merox Extraction Units a small heater or exchanger is provided to heat the rich caustic
before it enters the oxidizer. Although the oxidizer temperature should always be kept
as low as possible, the caustic temperature at the oxidizer inlet will normally be 100-
110°F (38º-43°C).
The oxidizer temperature should always be as low as possible while still maintaining
the desired degree of mercaptan regeneration. Operation above 120°F (49°C) must
be avoided to minimize corrosion of carbon steel.
Some Merox units are designed to extract very high levels of mercaptans (multi- 1,000
to over 10,000 wppm levels). In such cases, a high exothermic reaction across the
Oxidizer is expected due to the high quantity of mercaptides in the circulating caustic.
To minimize the delta T across the Oxidizer, a slipstream of lean caustic may be
recycled back to the inlet of the Caustic Heater via a spillback line from the Caustic
Circulation pump. This recycle stream is referred to as quench caustic. In extreme
cases of rich caustic with very high mercaptan loadings, a cooler may also be added
to the lean caustic downstream of the Disulfide Separator to reduce the amount of
quench caustic required. This stream dilutes the concentration of mercaptides by
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increasing the total volume of caustic and thus reduces the exotherm across the
Oxidizer. At times, the steam supplied to the caustic heater may be discontinued to
avoid high temperatures across the Oxidizer, assuming proper caustic regeneration
can be maintained.
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6.3.1 PROCESS FLOW OVERVIEW
The Merox extraction unit may be a gas phase or liquid phase extractor. However the
unit will typically include a Caustic Prewash and an Extractor. Regardless of the type
of extractor, the conventional regeneration system will have an Oxidizer and Disulfide
Separator at the minimum. This can be seen in Figure IV-1
Mercaptan-rich caustic solution from the bottom of the extraction section flows to the
regeneration section. Here, the stream is heated and air is injected before the
combined stream flows to the Oxidizer where the mercaptans in the caustic are
oxidized and converted to disulfide oils. From the Oxidizer, the caustic, disulfide oil,
proceed to the Disulfide Separator. Spent air is vented, usually to a fired heater within
the refinery; disulfide oil is withdrawn and sent to disposal or another process unit as
part of the combined feed to a hydrotreater or FCC Unit; regenerated (lean) caustic is
circulated back to the Extractor vessel.
Merox WS-2 catalyst is added periodically to enable mercaptan conversion to disulfide

oils in the regeneration section of the unit.
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Figure IV-1
Merox Extractor Plus Unit
1. Regeneration Section
The mercaptan-rich caustic solution containing dispersed Merox WS-2 Reagent

catalyst is withdrawn from the bottom of the Extractor vessel and sent to the
regeneration section of the unit. The mercaptan-rich caustic is heated slightly and
injected with a controlled amount of air upstream of the Oxidizer. The resulting catalytic
reaction converts the aqueous soluble sodium mercaptide to oil soluble disulfide oils
that are relatively insoluble in the caustic solution. The mixed phase of air, caustic and
disulfide oil then flows to the Disulfide Separator where they are separated.
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If the unit includes wash oil that is heavy gasoline or higher boiling points, it is injected
upstream of the oxidizer vessel to increase removal of disulfide in the disulfide
separator. The addition of oil decreases the specific gravity of the wash oil and
increases the rate of separation between the oil and caustic phases.
The first separation occurs between vapor and liquid in the Disulfide Separator Stack.
This allows the oxygen depleted spent air to be sent to disposal, the vented air has a
foul odor due to the presence of disulfide vapors. There may also be a small amount
of unreacted mercaptans and/or residual hydrocarbon present in the spent air. In
typical operation, the spent air mixture flows through a Vent Tank and two detonation
arrestors to a fired heater or incinerator. Spent air lines are hydraulically designed so
that the velocity either through them or a set of restriction orifices is high enough to
minimize the possibility of spent air flame backflash. Detonation arrestors must be
properly installed and kept in good working condition to arrest backflow should a
backflash occur.
The spent air has a significant amount of disulfide associated with it and can contribute
to the SOx emissions of the refinery upon incineration. Some designs may have a
Spent Air Scrubber to meet limits for the refinery. These scrubbers consist of a packed
bed with the spent air flowing upward countercurrent to a fresh heavy wash oil. The
wash oil absorbs the disulfide oil in the spent air and is sent to the Disulfide Separator
Stack for disposal with the Washoil/DSO through the Disulfide Sand Filter.
A second separation is then affected between the regenerated caustic and the
disulfide oil in the main body of the Disulfide Separator. This portion of the vessel has
a coalescing zone, comprised of anthracite coal crushed and screened to fall between
the #4 and #8 ASTM mesh, followed by a gravity settling zone. Upon separation, the
disulfide oil is periodically (or continuously) withdrawn to disposal as an upper oil
phase. The bottom regenerated caustic phase, containing a slight amount of dissolved
disulfide, is recirculated to the Extractor to complete the caustic loop.
The Disulfide Separator system design includes equalization lines to remove pockets
of gas that may form in the Disulfide Separator horizontal section, either through
emulsions or loss of stack level during an upset condition. During normal operations,
the equalization lines will also degas dissolved spent air from the liquid to prevent gas
pocketing in the disulfide oil transfer line and in the Disulfide Sand Filter. In both
scenarios, the spent air will transfer back to the Disulfide Separator stack to sustain a
hydraulic balance between the stack and disulfide oil transfer line.
Without the three equalization lines, gas pockets will form in the Disulfide Separator
horizontal section (anthracite coalescing zone), at the disulfide withdrawal piping at
the Disulfide Separator horizontal section, and at the top of the Disulfide Sand Filter.
This may result in accelerated corrosion in gas-pocketed sections and inability to
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transfer disulfide oil from the Disulfide Separator to the Disulfide Sand Filter. Figure
IV-4 below shows the equalization line system.
Figure IV-2
Disulfide Sparator Equalization System
Some feeds contain large amounts of mercaptans or contain more branched and
longer chain mercaptans. These mercaptans are more difficult to extract from
hydrocarbon streams. Examples of these feeds can be Coker LPG, gas plant C4, or
C5 streams. In these cases increased caustic circulation rates are required to remove
a sufficient quantity to make the mercaptan specification for the product. Sine caustic
circulation rate is increased, reentry sulfur increases proportionally. In these cases a
wash oil system is needed to reduce the disulfide oil in the caustic and ultimately in
the product.
The Single Stage Wash Oil is the least complicated version and removes a portion of
the disulfide oil from the caustic by injecting treated heavy gasoline or kerosene into
the rich caustic line upstream of the Oxidizer. This blends with the disulfide oil
generated in the oxidation of sodium mercaptide and reduces the blended specific
gravity, making the gravity separation more efficient.
The Two Stage Wash Oil injects a wash oil into the lean caustic upstream of the
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Caustic Circulation Pumps. The caustic/Washoil blend mixed in the pump for good
contact and then separates in the Wash Oil Settler. Lean caustic leaves the Wash Oil
Settler with about 50 wppm disulfide sulfur in the lean caustic. The wash oil blend is
skimmed off the top layer in the Wash Oil Settler and a portion is sent back upstream
of the caustic to mix with the fresh wash oil and caustic for better mixing. The other
portion is sent back upstream of the Oxidizer to act as a one stage wash oil and for
disposal through the Disulfide Separator and Disulfide Sand Filter. This system is not
offered for design at this time. It has been replaced by the more efficient Disulfide
Scrubber.
For those systems that require maximum caustic circulation and maximum flexibility in
their treating solution, the Disulfide Scrubber is located downstream of the Disulfide
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Separator, and acts as a multi-stage wash oil system for the removal of dissolved
disulfide oil in the lean caustic, resulting in minimal re-entry sulfur into the extractor.
Fresh wash oil enters the Disulfide Scrubber from the bottom, and flows upward across
packing, counter currently contacting the regenerated caustic from the Disulfide
Separator. Lean caustic with very low content of disulfide leaves the bottom of the
disulfide scrubber and returns to the Extractor, while the disulfide rich wash oil leaves
from the top of the disulfide scrubber. The disulfide rich wash oil stream is then sent
to either directly to a dedicated Disulfide Sand Filter, in the case of C3 or C4 used as
wash oil, or the inlet of the Oxidizer, enhancing the separation between caustic and
wash oil/disulfide oil blend.
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6.3.2 CONTROL PHILOSOPHY
Rich caustic flow from the Extractor to the Oxidizer is cascaded off of the level
controller on the air-liquid interface of the Disulfide Separator stack. The bottom of the
Extractor acts as the surge volume for the contents of the circulating caustic. This is
because the volume of caustic residing at the bottom of the extractor will change due
to dilution from water created in the mercaptan oxidation reaction and actual inventory
of caustic across the trays. It can also be controlled using a level controller at the
bottom of the Extractor. This is the case when two or more extractors share the same
caustic regeneration section.
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The caustic heater outlet and Oxidizer outlet temperatures may be controlled using a
low signal selector to select the temperature control location. Caustic flow to the
regeneration section is heated to 105º-110 F (40.5º-43°C). The primary controller is
the caustic heater outlet, which will adjust the steam flow to maintain the required
temperature to start the mercaptan oxidation reaction. However, if the exothermic
reaction causes the Oxidizer outlet temperature to be greater than 120°F (49°C), that
controller will reduce the steam flow to the heater (For KCS metallurgy in vapor phase
piping). If the unit has stainless steel (316L) metallurgy, the outlet temperature max is
set at 130º (54oC)..
A regeneration caustic circulation pump spill back controller may be designed to meet
pump minimum flow requirements, or lower the circulating caustic temperature rise
across the oxidizer, referred to as quench caustic. The quench caustic is reintroduced
upstream of the oxidizer.
The optimum caustic-hydrocarbon ratio that produces the minimum total sulfur in the
product is specified by UOP and a control valve on the lean caustic to the extractor is
used to maintain the desired flow of caustic. It should be noted that the caustic-
hydrocarbon ratio is designed to increase when feed rate decreases, thus the absolute
caustic circulation rate does not typically change with feed flow rate changes.
Plant air flow is controlled using a flow controller on the plant air inlet. The controller
uses measurements from an oxygen analyzer located on the spent air outlet to
maintain the required plant air flow. When the oxygen concentration of the spent air is
outside the typical 9-12 wt% range, the air control valve will open or close more to
manipulate the fresh air rate to the regeneration section.
During normal operations, spent air is routed to a vent gas tank and then to the fire
box of a heater. In case of an emergency, spent air from the vent tank can be diverted
to atmosphere by closing a valve on the spent air flow to the heater and opening a
valve on the vent tank vent line to atmosphere. Any caustic carried over or water that
condenses out of the spent air collects at the bottom the vessel and is disposed of on
level control.
The following diagram illustrates our current vent gas control scheme.
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Figure IV-3
Typical Vent Gas Control Scheme
The Merox reagent, Merox WS-2, must be regularly added to the regeneration caustic
to catalyze the conversion of sodium mercaptides to disulfide oil. Merox WS- 2 is
injected using a small proportioning pump, during programmed time intervals,
providing excellent catalyst distribution into the circulating caustic inventory. This
injection time can be optimized by increasing or decreasing the time intervals between
injections.
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6.4 TROUBLESHOOTING
Troubleshooting of any process, should be an ongoing part of normal operations. Daily

records of operations are collected and should be reviewed to observe 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. This section is
focused on process related problems such as poor product quality or contamination
and operating problems for unique equipment. Troubleshooting of general equipment
such as pumps, compressors, and heat exchangers is not included since this
information is generally available from the equipment vendors.
6.4.1 REGENERATION
Insufficient mercaptans oxidation may be attributed to:
1) Insufficient Air
2) The vented gas from the Disulfide Separator stack should be analyzed to
ensure that the O2 ranges between 9  12 vol%. Another method to check for
sufficient air injection is the Shake Test.
3) Low Oxidizer Temperature
4) The Oxidizer inlet temperature should not be below 100º F (38º C).
5) Insufficient Catalyst
6) If a regular catalyst addition is not followed, the catalyst concentration in the
circulating caustic may drop too low to promote adequate oxidation of
mercaptides. The Shake Test may be used to ascertain if catalyst is sufficient
or not.
7) Presence of Sulfide
8) The sulfides in the circulating caustic should be zero.
H2S Breakthrough to Extractor – If hydrogen sulfide is present in the feed to a Merox

Unit, it will react with caustic to form sodium sulfide.
H2S + 2NaOH  Na2S + 2H2O (1)
Sodium sulfide, derived from H2S breakthrough or sulfidic caustic carryover from the
Caustic Prewash, can then be expected to oxidize according to the following reactions
to form sodium thiosulfate and sodium sulfate:
Na2S + O2 + 1/2H2O  1/2 Na2S2O3 + NaOH (2)
1/2 Na2S2O3 + NaOH + O2  Na2SO4 + 1/2 H2O (3)

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Na2S + 2O2  Na2SO4 (4)
This formation of sodium sulfate or sodium thiosulfate is most common in Merox

Extraction units because feedstocks that are most amenable to mercaptan extraction
are also the most likely to contain H2S. Sodium sulfides present in Merox regeneration
section pose the following problems:
a. Caustic is consumed irreversibly
When sodium thiosulfate is produced, each mole of H2S sulfur consumes one
mole of sodium hydroxide. This is equivalent to 1.25 lb NaOH consumed for
each lb of H2S sulfur.
b. Oxygen requirements increase substantially
The stoichiometric or theoretical oxygen requirement for sodium sulfide

oxidation is four times that of sodium mercaptide oxidation when sodium
thiosulfate is produced, and eight times that of sodium mercaptide oxidation
when sodium sulfate is produced. Thus, air injection capability can very quickly
become the limiting factor in caustic regeneration.
c. The presence of sulfide suppresses mercaptide oxidation
It is necessary to essentially completely oxidize the sulfides before good

mercaptide oxidation can be attained.
d. The oxidation kinetics are significantly slower for sulfide than for mercaptide
The mercaptan oxidation may be inadequate since a large amount of sulfides

may not be oxidized completely on the first pass through the Oxidizer.
Sodium sulfate or thiosulfate, thus produced, remains in the aqueous phase. These
are neutral salts that deplete alkalinity needed for mercaptan extraction and increase
the salting out effect. If these salts are left to accumulate, their solubility limits could
be exceeded leading to crystalline precipitation and possible plugging.
The presence of sulfides in the regenerated caustic may interfere with the
potentiometric determination of mercaptan sulfur.
Sulfide contamination is easily detected by testing the rich caustic with lead acetate
paper or solution. The sulfides present in the circulating caustic must be addressed
promptly by checking the operation and performance of the prewash. Increasing the
catalyst concentration, oxidizer temperature, and air rate may be used to speed up the
elimination of sulfide interference.
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If sulfide contamination has been severe, for reasons discussed above, some or the
entire caustic inventory may require replacement.
6.4.2 OTHER TOOLS TO CHECK

HE CAUSTIC REGENERATION SECTION
6.4.2.1 Shake Test
The "shake test" is a simple method that can be used at the unit by the operators to
estimate the effectiveness of Merox caustic regeneration.
Procedure:
Half fill a small, clear glass bottle with regenerated Merox caustic solution taken after
the disulfide separator. The color of the solution should be dull green or greenish blue.
Stopper the bottle and shake vigorously. The color of the solution should change to a
bright green or deep blue within two minutes of shaking.
If more than two minutes of shaking are required to make the color change, either
insufficient air is being injected to the oxidizer, the oxidizer temperature is too low, or
there is insufficient catalyst in the caustic. If less than 30 seconds of shaking is required
to make the color change, either excessive air is being injected, the oxidizer
temperature is too high, or there is an excessive amount of catalyst in the caustic. A
deep blue solution when the sample is taken indicates that there are no mercaptides
remaining in the regenerated caustic. In this case, dissolved oxygen could be carried
back to the extractor, allowing disulfide formation in the extractor as mentioned before.
NOTE: This test may be impractical when the caustic is heavily discolored, muddy,
murky, and contains a high concentration of thiosulfate as a result of sulfides
contamination.
6.4.2.2 Disulfide Separator Vent Gas
The oxygen content of the vent gas can be helpful when troubleshooting unit
performance. Oxygen content below 9% would indicate inadequate air injection,
excessive oxidizer temperature, or presence of sulfide. Oxygen content above 12%
indicates excessive air injection, inadequate oxidizer temperature, or inadequate
catalyst concentration in the Merox caustic.
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6.4.3 DISULFIDE SEPARATION

If the disulfide oil separation is poor, there will be re-entry of disulfides into the
hydrocarbon. If this is suspected, the regenerated caustic from the disulfide separator
should be checked for disulfide oil content, using UOP Method 393.
6.4.4 EMULSIFICATION AND CAUSTIC ENTRAINMENT
Merox catalyst in caustic solution does not increase the tendency of caustic solutions
to emulsify with hydrocarbons, but strong salts do. Scale and dirt will be almost
completely dislodged by Merox caustic. Finely divided suspended material can
stabilize emulsions. It may be necessary to discard the first batch of caustic during the
startup if caustic picks up a big load of scale and dirt from used equipment. Part of this
scale and dirt may be iron sulfide.
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This section covers the procedures that are unique to the operation of the Caustic
Extraction Merox Unit.
6.5.1 DISULFIDE SAND FILTER BACKWASHING
As contaminants or impurities collect in the sand bed, it will lose its coalescing
efficiency and the differential pressure across the sand filter will gradually increase.
Initially the differential pressure across the filter will be negligible (near indiscernible).
When a differential pressure is apparent, as indicated by a difference of >14 kPa (>2
psi), the sand filter should be taken out of service for backwashing. Failure to do so
will result in continued differential pressure buildup and will lead to mechanical failure
of the sand support screen and inefficient coalescing of hydrocarbon impurities.
Backwashing should be conducted as follows:
a. Open the hydrocarbon line bypassing flow around the sand filter vessel and
block in the Sand Filter, including the equalization lines.
b. Pump out or drain the remaining hydrocarbon from the vessel. Displace the
hydrocarbon with steam or inert gas while taking the necessary precautions to
ensure that the vessel is maintained under a slight positive pressure at all times.
c. Open the backwash line provided at the sand filter inlet line, removing the blind,
if provided.
d. Connect a temporary water supply to the connection provided at the vessel
drain.
e. Begin filling with water.
f. When the vessel is full of water, flush at a vigorous water flow rate, upflow
taking care that no sand is floated out the inlet.
g. The backwashing may be considered complete when the effluent is essentially
clear and free of suspended matter.
h. Put Sand Filter back into service, using safe refinery practices.
6.5.2 OXIDIZER LOADING INSTRUCTIONS
Prior to starting loading the Oxidizer, confirm that a sufficient amount of 40 mm (1½")
Diameter Carbon Raschig Rings are available for loading.
a. Verify that the Oxidizer is completely blinded and isolated, except for the drain.
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b. Verify that a final closure has been performed on the 8” blankoff on the Oxidizer.
c. Install a blind at the gate valve on the pumpout line from the Oxidizer to the
Caustic Circulation Pumps.
d. Verify that the gate valve on the Oxidizer bottoms line to the open drain is
closed.
e. After the Oxidizer is mechanically complete, open the top manway (or top
head).
f. Verify that the Oxidizer is clean inside and that no garbage was left in the
vessel or drain. Check the nozzle weld bars.
g. Fill the Oxidizer with clean water (meets Merox water quality standards) until
the level is just below the neck of the manway.
h. Carefully begin adding the Raschig Rings through the manway, minimizing the
amount of rings that are damaged, and maintaining a water level just below
the neck of the manway.
i. Fill the Oxidizer with Raschig Rings to a level flush with the flange, making
sure the entire vessel is filled and avoiding a coning effect.
j. When the loading is completed, drain the water. After all the water is removed,
the level may fall and more rings may need to be added to maintain the level
flush with the flange.
k. Fill the bed again and then rinse the bed of fines.
l. When finished draining the vessel of water, close the manway. Verify that the
2" utility connection on the Oxidizer outlet is closed.
6.5.3 OXIDIZER UNLOADING PRECAUTIONS
When the refiner wishes to open the Oxidizer for maintenance and/or inspection
purposes, care must be taken to remove any hazardous chemicals and or
hydrocarbons prior to opening the vessel. UOP recommends that the vessel and
internals be very thoroughly rinsed with water to flush out the caustic (most simply
indicated by a reduction in pH of the waste water). Only after full safety procedures
have been followed, should the side and top manways be opened for removal of the
Raschig rings.
6.5.4 DISULFIDE SEPARATOR LOADING INSTRUCTIONS
Prior to starting the loading of the Disulfide Separator, confirm that a sufficient amount
of screened 4-8 Mesh Anthracite Coal and 40 mm (1½") Diameter Carbon Raschig
Rings are available for loading. The coal may need to be screened at site if it contains
greater than 5% fines.
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a. Verify that the following vessel blinds are installed:

• Vessel Inlet Line Flange.
• At the gate valve on the Oxidizer pumpout line to the Caustic Circulation
Pumps.
• Stack outlet equalization line to/from the Disulfide Sand Filter.
• Main Body disulfide outlet/level glass line at the top of the vessel.
• Main Body level glass, lower nozzle connection to vessel.
b. Verify that the lines leading to and from the Separator Stack level glass and
level transmitter are closed. Isolate the main body level glass.
c. Verify that the isolation valves around the flow control valve for the caustic inlet
to the Extractor are closed.
d. Close the two gate valves on the Caustic Circulation Pumps discharge
minimum flow line to the Disulfide Separator.
e. Confirm that the 2” gate valve from the Disulfide Separator to the open drain
is closed.
f. Verify that the Circulating Caustic Sampling Station is closed.
g. Confirm that the Caustic Circulation Pumps are valve isolated at the suction
and discharge.
h. After the Disulfide Separator is mechanically complete, open the top and side
manways.
i. Verify that the Disulfide Separator is clean inside and that nothing was left in
the vessel. Inspect internal screens.
j. Perform a final closure with the proper gasket on the side manway.
k. Confirm that a final closure with the proper gasket has been performed on the
6” unloading blankoff on the bottom of the coalescing zone.
l. Fill the Separator with clean water until the level is approximately 200-300 mm
(8-12 in) below the neck of the manway.
m. Prior to loading the anthracite coal, it is recommended sieving it manually or
using sieving system with a number 8 sieve per ASTM Specification E11 to
remove fines. The number 8 sieve has openings of approximately 2.4 mm
(3/32 inch) square.
n. Carefully begin adding the coal through the manway, maintaining a water level
just below the neck of the manway. Drain water as necessary to keep a level
just below the neck of the manway.
o. Special attention should be given to getting an even bed of coal to the top. It
is critical that the area in the upper corners are also filled with coal. This can
be done using a clean, long wooden plank to push the coal in the corners. No
void areas should be present anywhere in the coalescing zone. Be careful: If
you push too hard, you may rupture that support screen.
p. To account for settling, fill the neck of the manway completely, flush with the
flange.
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q. When the loading is completed, drain the water through the drain at the
separator bottoms outlet line. Make sure any lines that were inadvertently filled
with water are also drained. After all the water is removed, the level may fall
and more coal may need to be added. For vessels with a diameter larger than
5 feet, refill the main body portion of the vessel with water again and drain
quickly. If level of coal slumps again, add more coal.
r. Perform a final closure on the loading manway with the proper gasket.
s. Open the manway at the top of the Separator Stack. Make sure that the
packing support is in place. Check the nozzle weld bars.
t. Fill the stack with carbon Raschig Rings as high as possible without interfering
with the closure of the manway. Take care to avoid breakage of the rings.
u. Perform a final closure on the manway with the proper gasket.
6.5.5 DISULFIDE SEPARATOR UNLOADING

PRECAUTIONS
When the refiner wishes to open the Disulfide Separator for maintenance and/or
inspection purposes, care must be taken to remove any hazardous chemicals and or
have been followed, should the top manways be opened for removal of the anthracite
coal and Raschig rings.
6.5.6 VENT TANK LOADING INSTRUCTIONS

Prior to starting the loading of the Vent Tank, confirm that a sufficient amount of 40
mm (1½") Diameter Carbon Raschig Rings are available for loading.

• Vessel Inlet Line Flange
• Vessel Drain Line Flange
b. Verify that the lines leading to and from the level glass are closed.
c. After the Vent Tank is mechanically complete, open the top manway. Check
the nozzle weld bars.
d. Verify that the Vent Tank is clean inside and that no garbage is on the support
grid.
e. Make sure that the packing support is in place.
f. Fill the Vent Tank Drum with Raschig Rings as high as possible without
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interfering with the closure of the manway.

g. Level the Raschig Rings and close the top manway.
h. Note the quantity of Raschig rings loaded for future reference and complete
the loading diagram.
6.5.7 VENT TANK UNLOADING PRECAUTIONS

When the refiner wishes to open the Vent Tank for maintenance and/or inspection
purposes, care must be taken to remove any hazardous chemicals and or
have been followed, should the top manways be opened for removal of the Raschig
rings.
6.5.8 DISULFIDE SAND FILTER LOADING INSTRUCTIONS

Prior to starting the loading the Disulfide Sand Filter, confirm that a sufficient amount
of quartz silica 8-16 mesh sand is available for loading.

• Vessel Inlet Line Flange
• Vessel Outlet Line Flange
• Vessel Drain Line Flange
• Vessel Outlet to Top of Disulfide Separator
b. Verify that the lines leading to and from the level glass are closed.
c. After the Disulfide Sand Filter is mechanically complete, open the top manway.
d. Verify that the Disulfide Sand Filter is clean inside and that no garbage is on
the grid.
e. Tightly cover the distributor slot with a plastic tarp or other suitable material to
prevent sand from entering the distributor.
f. Begin adding sand. Add enough sand to cover the support by 2 to 4 inches.
Confirm that the sand has not leaked through.
g. Once the support has been determined to be stable, perform a final closure on
the side manway and continue loading sand from the top manway. Level the
sand once the sand nears the top and measure the distance from the middle
of the distributor to the top of the bed.
h. Fill the sand until the level top of the bed is approximately 70 mm (3") below
the center of the distributor, or as specified in the vessel drawing of the
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Schedule A. Make sure the bed is leveled.

i. When the loading is completed, uncover the distributor and close the top
manway with the proper gasket installed.
Note the quantity of sand loaded for future reference and complete the loading
diagram.
6.5.9 DISULFIDE SAND FILTER UNLOADING

PRECAUTIONS
When the refiner wishes to open the Disulfide Sand Filter for maintenance and/or
have been followed, should the top manways be opened for removal of the sand.
6.5.10 DISULFIDE SCRUBBER LOADING INSTRUCTIONS
Note: Refer to the UOP Schedule A Project Specifications (# 301 for

the vessel and 307 for the packing specs)
Prior to starting the loading of the Disulfide Scrubber, confirm that the Packing Material
and Inlet Distributor and distributors of the packing in between are available for loading.
The loading will start from Bed No. 3 (bottom bed) and move up to Bed No. 1 (top bed).
Note that this could be a plate that is perforated and need to place in opposite order
or staged order.
1) Initially the vessel will need to be taken apart at the body flange just above Bed
No. 3. This will require the following to be blanked off:
a) 2” Vessel Wash Oil Inlet Line Flange

b) 2” Vessel Caustic Outlet Line Flange
2) Verify that the line leading to and from the level glass LG- are closed.
3) After the Disulfide Scrubber is mechanically complete and the Coalex
Coalescer has been installed properly, open the body flange above Bed No. 3.
Check the Coalex Coalescer with a boroscope; the coalex has a darker color
at the top layer. Check the distributor orientation and size.
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4) Verify that Bed No. 3 is clean inside and that no garbage is on the support grid.
5) Make sure that the packing support is in place. Fill the Bed with Packing
Material as high as possible without interfering with replacing the bed limiter
6) Replace internal components and ensure distributor is properly installed. Close
the body flange. Note that you need to see how the distributor is and if a
perforated plate need to be placed staggered in between.
7) Open body flange just above Bed No. 2.
Material as high as possible without interfering with replacing the bed limiter
the body flange. Check distributor orientation and size.
11) Open body flange just above Bed No. 1.
Material as high as possible without interfering with replacing the bed limiter.
the body flange. Check distributor orientation and size.
Refer to the Schedule A vessel drawing and packing information.
6.5.11 DISULFIDE SCRUBBER UNLOADING PRECAUTIONS
When the refiner wishes to open the Disulfide Scrubber for maintenance and/or
have been followed, should the top manways be opened for removal of the packing.
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7. PROPYLENE RECOVERY UNIT

7.1 INTRODUCTION
7.1.1 SCOPE
UOP issues this General Operating Manual (“GOM”) to provide background process
information to the engineering group of the operating company or detail design
engineering contractor (“Contractor”) as an aid to the detailed design activities and
development of operating procedures and practices. The GOM is not considered a
part of the Project Specifications but they do provide information related to the
specifications included in the Schedule A. This material is informational purposes only
and is intended to augment the information provided in Project Specifications. This
information is expected to be reasonably consistent with the Project Specifications; it
may not represent exact consistency with the Project Specifications. Any major
inconsistencies should be brought to the attention of UOP for clarification. In all
situations, the information provided in the Project Specifications takes precedence
over information in the GOM. Accordingly, UOP assumes no responsibility for the mis-
application of this information to a specific process, particularly the use of such
information to prepare detailed operating instructions for a specific process.
7.1.2 PURPOSE
The UOP Propylene Recovery Unit (PRU) separates and treats a mixed C3/C4 stream
from the Unsaturate LPG Merox Unit, which is downstream of the Gas Concentration
Section of a Catalytic Cracking Unit, to produce high purity propylene (99.5 wt-%
minimum) for use in polypropylene production. Within the PRU, propylene can be
treated to remove trace amounts of Carbonyl Sulfide (COS), Water, Arsine, Phosphine
and Antimony. Also produced are the propane and C4 streams for additional
downstream processing.
The LPG feed first enters a C3/C4 Splitter to remove butanes and butenes for further
downstream processing. The C3/C4 Splitter overhead mixture of propane and
propylene is sent to either the Deethanizer to remove ethane and lighter compounds,
or directly to C3 Splitter.
Deethanizer may be or may not be part of the design depending on the C2-
specification of the propylene product. This manual assumes that there is a
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Deethanizer column downstream the C3/C4 Splitter overhead. Net off-gas from the
Deethanizer Receiver is recycled to the Gas Concentration Section of the Catalytic
Cracking Unit. The hydrogen sulfide that may come with the feed to PRU will be
stripped in the Deethanizer. The mixed C3 stream from the bottom of the Deethanizer
is fed to the C3 Splitter.
The mixed C3 stream must be fractionated into propane and propylene. Propane is
sent from the bottom of the C3 Splitter and can be combined with the C4 material from
the C3/C4 Splitter. Propylene from the overhead of the C3 Splitter is further treated
downstream. The separation of propylene from propane by distillation is very difficult.
A large number of trays operating at a very high reflux rate would be needed to make
this separation in a conventional column. Therefore, three special technologies are
available for use in this fractionator.
1. A Heat Pump Compressor System (HPC) is used instead of the conventional

reboiler and condenser. It allows low pressure fractionation of propylene from
propane. The overhead vapor flows into a Compressor Suction Drum, to a heat
pump compressor, to the C3 Splitter Reboilers and returns to the C3 Splitter.
The overhead vapor is heated via compression and is used to reboil the
column. After cooling and condensing, the overhead material combines with
the overhead liquid from the Compressor Suction Drum and returns to the
column as reflux. This assures that there is adequate reflux to give the desired
separation of propylene from propane.
The heat balance of the C3 Splitter must be maintained, so excess heat input
from the Heat Pump Compressor must be removed by the Trim Condenser. A
slip stream of overhead vapor from the Heat Pump Compressor is sent to the
C3 Splitter Trim Condenser where it is condensed and returned to the
Compressor Suction Drum. The flow is controlled to maintain pressure in the
Compressor Suction Drum, as more vapor is condensed the pressure will drop.
Low pressure distillation is desirable because the relative volatility (i.e. ease of
separation) between propylene and propane is greater at low pressure. In
practice, this means fewer distillation trays operating with less reflux. This
allows the construction of a smaller column (height and diameter), and a
smaller reboiler/condenser.
2. The second special technology is UOP MD distillation trays which are low
profile, multiple downcomer trays that allow the column height and diameter to
be reduced. Compressor horsepower is also reduced because MD trays
operate with less pressure drop than conventional trays.
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3. The third special technology is UOP High Flux Tubes. This tubing reduces the
size of the reboiler/condenser by promoting more efficient heat transfer
between the overhead and bottoms material.
Typically the trace moisture is present in the PRU feed that comes from the LPG Merox
Unit which tends to drive the C3= product off spec. Therefore the C3 Splitter overhead
stream is routed through a set of Molecular Sieve Driers to remove water.
Depending upon processing requirements and feed quality, the carbonyl sulfide and
trace metal removal system may or may not be included in the unit design. The dried
propylene can be processed through the set of Activated Alumina Treaters to remove
the COS in case the COS content in the C3 Splitter overhead exceeds the specification.
Special metal oxide based adsorbent can also remove the trace metals such as Arsine,
Phosphine (and any other metals present). The latest design approach is the
combined COS and trace metal removal system which is comprised of GB series metal
oxide based adsorbent beds. This manual assumes this type of design.
The high purity propylene is sent to Intermediate Storage and ultimately to a

Polypropylene Plant for further Processing. Depending upon processing requirements,
the propylene may be sent to a UOP Selective Hydrogenation Process to saturate
dienes and acetylenes.
7.1.3 BLOCK FLOW DIAGRAM
Refer Figure I-1 for the General flow scheme of the Propylene Recovery Unit.
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Figure I-1
PRU Flow Scheme
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7.2.1 PRU PROCESS VARIABLES
7.2.1.1 Feed Quality
The composition of the feedstock to the UOP Propylene Recovery Unit is determined
by the severity of the operation in the upstream Catalytic Cracking Unit and the type
of feedstock sent to the Cracking Unit. The more severe the operation of the Catalytic
Cracker, the greater the production of olefins. As the proportion of hydrotreated
material in the Catalytic Cracker increases, the olefin content of the products will be
reduced. This reduction of olefins is due to the larger amount of hydrogen in the feed
and the hydrogen transfer reactions which occur as a result. The fluctuating olefin
concentration sent to the PRU will affect the fractionation quality. The C3 Splitter has
been equipped with multiple feed nozzles in order to maintain the desired product
quality when the olefin concentration of the feed is changing.
Also, the amount of COS and other contaminants to be removed by the PRU will be
determined by the feedstock and the severity of the operation on the Catalytic Cracker.
7.2.1.2 Feed Rate
A change in the feed rate changes the heat duty on all of the fractionation exchangers
as well as the vapor/liquid loadings of the fractionation towers themselves. Operating
at a LHSV above design risks overloading of the driers and/or treater(s) and eventual
contamination of the propylene product.
7.2.1.3 C3/C4 Split
The C3/C4 Split is determined by controlling the top tray temperature with the quantity
of reflux sent to the tower. The control objective is to minimize the loss of C3‘s to the
C4 stream as this is a loss of yield. Typically, there will be a small fraction of iso-butane
and n-butane in the overhead product.
7.2.1.4 Deethanizer Product Quality

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The reboiler duty in the Deethanizer will determine the quality of the C3 stream to be
sent to the C3 Splitter. If the reboiler rate is too low, C2‘s will pass through to the C3
Splitter and will reduce product purity and possibly cause a non-condensibles problem
in the C3 Splitter. If the reboil rate is too high, valuable C3‘s will be sent overhead. The
Deethanizer net overhead vapor is recycled to the Gas Concentration Unit where the
C3‘s are removed and returned to the Propylene Recovery Unit.
7.2.1.5 Propylene Purity
The purity of the propylene produced is determined by its application. Chemical Grade
Propylene has to be 95 wt% pure. Polymer Grade has to be 99.5 wt% pure. The
product purity is monitored by checking the purity of the overhead liquid from the C3
Splitter with an on-line analyzer. To maintain the desired purity, the reboil rate of the
tower is manipulated by changing the amount of hot overhead compressor discharge
gas which is sent through the reboiler.
7.2.2 FRACTIONATOR PROCESS VARIABLES
7.2.2.1 Material Balance
If sufficient time is given to come to a steady state, all fractionating columns will heat
and material balance. The law of conservation of mass and energy requires:
Input - output = accumulation
For a steady state, there is no accumulation in a given system. This essentially means
that what goes in must come out. Both the mass and energy inputs must be equal to
outputs. Let us examine this concept with respect to fractionation.
The instrumentation for a fractionator must be designed such that the column material
balances, in order to establish a stable operation. To establish an overall material
balance, both overhead and bottom draw rates must be properly controlled. The
portion of the feed that is not taken out as overhead product must necessarily appear
as the bottom product or vice versa.
7.2.2.2 Heat Balance

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The heat balance is not independent of the material balance. The rate of vapor flow
up the column is a function of heat input at the bottom of the column and the heat input
at the feed point. Hence, any heat input by the reboiler and the feed stream must be
removed in the overhead condenser if the column is to heat balance. Of course, this
assumes negligible heat loss from the column to the environment.
Another aspect of the heat balance is the natural temperature profile in the column. In
order to obtain a good separation, the temperature profile must not be constrained. An
example of constraining the temperature profile would be to try to hold a tray at a
temperature lower than the boiling point of the material on that tray. This is a violation
of the heat balance, which is independent of temperature profile.
7.2.2.3 Product Control
1) Heat Input and Reflux
Heat input and reflux are the most important variables in distillation. The reflux is
directly related to the heat input because the vapor boiled up to the overhead receiver
must be returned to the column if it is not drawn off as overhead product. Most columns
are operated with a constant heat input. Figure II-1 graphically represents the effect of
reflux on product quality. The slope of the upper operating line is L/V in the upper
section of the column. If the heat added to the column is reduced, thus reducing the
L/V ratio, and if all other variables are constant, the operating line will approach the
equilibrium curve. The number of trays are fixed by column design. Hence, as reflux
is reduced, the overhead purity will decrease since the magnitude of rectification
(rectification occurs above the feed tray) per tray will drop. The same argument holds
true for the stripping section (below the feed tray) resulting in decrease in purity of the
bottoms. Conversely, if the heat input and reflux were increased, L/V will increase and
both the top and bottom product qualities will increase.
Even though the increase in reflux and heat input to the column increase the product
purities, it must be borne in mind that there is a limit. The limit is governed by "flooding"
of the column. The condition of flooding is said to have been reached when the
pressure drop of vapor across a tray is greater than the liquid head in the downcomer
or when liquid traffic through the downcomer is excessive. When a fractionating
column "floods" some of the vapor travels up the downcomer. Under such conditions,
proper fractionation of the components will cease and the product purities will be
adversely affected. The column then has to be unloaded by lowering the reflux rate
and heat input to put the column back into normal operation.
2) Feed Temperature
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Feed to the fractionating column is generally close to its bubble point temperature. If
the feed is at a temperature below its bubble point temperature, then the rectifying
section will be helped at the expense of the stripping section. This will result in higher
overhead purity and lower bottoms purity.
Conversely, if the feed is partially vaporized, then the stripping section will be helped
at the expense of the rectifying section. This discussion, of course, assumes that other
variables are held constant.
3) Pressure
In distillation, the column pressure is not an operating variable. This does not imply
that the degree of fractionation does not change with pressure. We simply mean that
under normal operation, the column pressure is held constant at its design pressure.
If the pressure is increased, the equilibrium will change, such that it is necessary to
add more heat to do the same fractionation. The control of the column pressure is
performed by a separate column overhead pressure control system. Once the required
pressure is attained, it should not be changed.
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7.3.1 C3/C4 SPLITTER (DF-21401)
The LPG to the UOP Propylene Recovery Unit (PRU) is first fed to the C3/C4 Splitter
(See Figure IV-1). This fractionates butanes and heavier components (C4+) from a
mixture of lighter components (mixed C3 and C2’s). The C4+ material from the bottom
of the Splitter continues on to other downstream processing.
There are two primary controls to adjust C3/C4 Splitter operation and thus the amount
of C4+ material in the propylene and propane products. They are the reboiler heat
input and the upper tray temperature. Other process parameters, such as pressure
and levels are not normally adjusted.
The feed rate to the Propylene Recovery Unit (PRU) is equal to the C3 and C4 LPG
production from the Gas Concentration Unit of the Catalytic Cracking Unit. The feed
rate to the PRU will vary as operation of the Catalytic Cracking Unit varies. The PRU
feedrate is adjusted automatically by the backpressure controller on the LPG feed
pump in the LPG Merox Unit.
Feed enters the C3/C4 Splitter column after being preheated with the C4+ material
leaving the bottom of the column. There are typically two reboilers provided for C3/C4
Splitter. The first reboiler heat input is supplied by circulating hot oil or heat integration
with upstream units (usually circulating stream from upstream FCC unit, such as LCP,
or heavy naphtha). The second reboiler is an “auxiliary” steam reboiler sized for 40 to
60% of reboiler duty. Steam reboiler is provided for flexibility in operations, especially
during the start-ups and shutdowns. The heat input is controlled to provide enough
vapor traffic up the tower so there is adequate reflux to give the desired C3-C4
separation. Reflux flow is controlled to hold a tray temperature stable near the top of
the column. This will keep the composition of the overhead material (mixed C3)
constant. The net overhead material is pumped to the Deethanizer to control the level
in the overhead receiver. The C3/C4 Splitter bottoms material is pumped out to storage
to control the level in the bottom of the column. A drag line is provided to vent non-
condensibles from the top of the overhead receiver.
7.3.1.1 Heat Input
Heat input to the reboilers is provided by hot oil, heat integration and/or low pressure
steam. The flowrate of the heating medium at the reboiler is controlled to provide
sufficient vapor-liquid traffic in the tower for good fractionation. As the reboiler heat
input is increased, more LPG boils overhead and reflux increases automatically, to
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maintain the set upper tray temperature. Thus, more reboiler heat input results in more
vapor-liquid contacting which increases the separation between the light (C3-) and
heavy (C4) streams. However, using more heat than necessary is uneconomical, and
the column will flood if an extreme amount of heat is used. Normally, heat to the
reboiler is set such that the reflux rate is close to design and the upper tray temperature
is adjusted to fine tune the composition of the overhead material.
7.3.1.2 Reflux Rate
The temperature controller located on an upper tray in the column is the main control
for holding the composition of the overhead product (C3-) stable, the controller is
cascaded to the reflux flow. This affects the component distribution in the column, not
the degree of separation. Tray temperature is set to give the maximum concentration
of C4 allowed in the overhead product. Decreasing this temperature will increase reflux
resulting in less C4 in the overhead product but more mixed C3 will be lost out the
bottom.
7.3.1.3 Overhead Pressure Control
Varying the tower pressure will change the composition of the overhead material (at a
constant upper tray temperature), but pressure is not usually used as an operating
control. Pressure is set at design conditions and left alone. It is important however that
this controller function well because stable column operation is impossible without
constant pressure. Column pressure is usually controlled by a hot-vapor bypass (see
Figure VI-1 and the sketch below). Column overhead pressure controller controls a
valve which regulates the flow rate to the overhead condenser. Differential pressure
(dP) controller is necessary to keep column pressure controller in its operating range
under the wide range of cooling conditions expected from an air cooled condenser.
The differential pressure controller regulates the flow of hot vapor to obtain a
temperature at the surface of the receiver liquid to give a vapor pressure to satisfy the
dP requirement.
There is a non-condensable vent lines included on each tube bundle of condenser.

Non-condensable material can vented to ensure proper operation of the pressure
controller. As the condenser outlet line should not be sealed with liquid but free-
draining to the receiver, there is also an equalizing line provided to allow hot vapor
from the receiver to get back to the condenser outlet and prevent formation of a liquid
leg with high static head:
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7.3.2 DEETHANIZER (DF-21402)
The Deethanizer fractionates ethane and lighter components (C2-) from a mixture of
propylene and propane (mixed C3). The C2- material from the top of the Deethanizer
is recycled to the Gas Concentration Unit.
The feed to the Deethanizer is on flow control from the C3/C4 Splitter overhead pumps.
The primary control to adjust the Deethanizer operation and thus the amount of C2
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material in the propylene and propane products is the reboiler heat input. Other
process parameters, such as pressure and levels, are not normally adjusted.
The reboiler heat input is supplied by low or medium pressure steam. The reboiler is
a horizontal stabbed-in reboiler. The flow of steam is controlled to provide enough
vapor traffic up the tower so there is adequate reflux to give the desired separation.
The total overhead liquid flow is refluxed back to the column. As the reboiler heat input
is increased more C2- boils overhead. The reflux increases automatically to maintain
the level in the overhead receiver. Thus, more reboiler heat input results in more vapor-
liquid contacting which increases the separation between the mixed C3 stream and C2-
off-gas. However, using more heat than necessary is uneconomical, and the column
will flood if an extreme amount of heat is used. Normally, heat to the reboiler is
adjusted to fine tune the composition of C2 in the bottoms material.
The net off-gas is sent to the Gas Concentration Unit on pressure control. Varying the
tower pressure will change the composition of the overhead material (at a constant
upper tray temperature), but pressure is not usually used as an operating control.
Pressure is set at design conditions and left alone. It is important however that this
controller function well because stable column operation is impossible without
constant pressure.
The waste water from the overhead receiver water boot is often sent to a degassing
drum and is set by the level controller of the overhead receiver level boot. The water
degassing drum is provided to vent any entrained LPG to the relief header prior to
sending the waste water for downstream treatment. The bottoms product is sent to the
C3 Splitter and regulated by Deethanizer bottoms level controller. Refer to Figure IV-
2.
7.3.3 C3 SPLITTER (DF-21403)
7.3.3.1 C3 Splitter Flows
Feed to the C3 Splitter is fractionated into propane and propylene. Propane is sent
from the bottom of this column to storage and propylene from the overhead of the
column is further treated downstream (See Figure IV-3).
The separation of propylene from propane by distillation is very difficult, as the

difference in the normal boiling points of propane and propylene in only 5.9°C:
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Normal boiling point Deg. C

Propylene -47.7
Propane -41.8
A large number of distillation trays operating at a very high reflux rate would be needed
to make this separation in a conventional column. Therefore, three special
technologies have been used in these fractionators that include the UOP MD
distillation trays, heat pump compressor (HPC) and special UOP High Flux Tubing.
Heat pump compressor process flows and controls are covered in this section. Heat
pump compressor provides two main benefits: elimination of the conventional
condenser and fractionation at low pressure.
The mixed C3 stream is fed one-quarter of the way up the column. Two additional
lower feed nozzles could be provided in case the composition of the mixed C3 feed is
expected to change. If the column feed content of propylene is reduced, a portion of
the column feed is directed to the lower feed nozzles. This must be done in order to
maintain the same degree of component separation. The overhead vapor flows into
the flash drum called Compressor Suction Drum and on to a heat pump compressor
and then to the C3 Splitter thermo siphon Reboilers. The overhead vapor is heated via
the compression and is used to reboil the column. After cooling and condensing in the
reboiler, the overhead material returns to the C3 Splitter by joining the reflux line as a
liquid. Because most of the overhead material is condensed in the reboiler it is possible
to eliminate the large overhead condenser needed for a conventional distillation tower.
The flow of overhead material from the reboiler is controlled to provide enough vapor
traffic up the tower so there is adequate reflux to give the desired separation of
propylene from propane. This is analogous to controlling the heat input to a reboiler
on a conventional distillation column.
The heat balance of the C3 Splitter must be maintained, so excess heat input from the
Compressor must be removed by the C3 Splitter Trim Condenser. A slip stream of
overhead vapor from the Compressor is sent to the C3 Splitter Trim Condenser where
it is condensed and returned to the Compressor Suction Drum. The overhead vapor
flow through the condenser controls the pressure in the Compressor Suction Drum.
As more vapor is condensed, the Compressor Suction Drum pressure will decrease.
The heat pump compressor allows the column to operate at low pressure while the C3
Splitter Trim Condenser operates at just high enough pressure to condense propylene.
Low pressure distillation is desirable because the relative volatility (i.e. ease of
separation) between propylene and propane is greater at low pressure. In practice,
this means fewer distillation trays operating with less reflux. This allows the
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construction of a smaller column (height and diameter), a smaller reboiler and a

smaller condenser.
Reflux is returned to the C3 Splitter to control a small concentration of propane

(measured by analyzer) on a tray in the top section of the column.
The level in the Compressor Suction Drum is maintained by the flow of overhead
product to propylene driers.
7.3.3.2 C3 Splitter Controls
There are two primary controls to adjust C3 Splitter operation and thus the amount of
propane in the propylene product. They are the reboiler heat input and the propane
analyzer-controller in the upper section of the column. Other process parameters, such
as pressure and levels are not normally adjusted. The control of this column is very
similar to a conventional column like the C3/C4 Splitter, even though the hardware is
quite different.
The feed rate to C3 Splitter is adjusted automatically by the bottoms level controller of
the Deethanizer.
1) Heat Input
Heat input to the two thermo siphon reboilers is provided by overhead material from
the Heat Pump Compressor discharge. This material is sent to the reboiler tube side
at a temperature higher than the liquids on the shell side thereby effecting boil up. The
liquids heated up on shell side along with the vapors entrained rise up the reboiler
return line and flash into the reboiler compartment of the C3 Splitter. The separated
vapors rise up the column providing vapor traffic.
The flow of overhead material from the reboilers is controlled to provide enough vapor-
liquid traffic in the tower for good fractionation. The condensed liquids exit out of tube
side of each reboiler. There are flow control valves at the exit of tube side of each
reboiler which are controlled independently by the flow control (FIC) loops. Increasing
the Set Point on FIC entails increased vapor circulation through the HPC and
accordingly increases the work done across HPC acting as a heat source. Both FICs
ideally are set at equal rates to distribute the heat load. Reboiler heat load and boil up
can be increased or decreased by changing the Set Points on the FICs.
To increase the vapor flow and compression through the HPC the operator has to
increase the load on the machine by increasing the RPM by speed control as
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necessary.
As the reboiler heat input is increased more LPG boils overhead and reflux increases
automatically to maintain the set upper tray composition (as controlled by propane
analyzer). Thus, more reboiler heat input results in more vapor-liquid contacting which
increases the separation between propylene and propane. However, using more heat
than necessary is uneconomical, and the column will flood if an extreme amount of
heat is used. Normally, heat to the reboiler is set so that the reflux rate is close to
design and the upper tray propane analyzer-controller fine tunes the composition of
the overhead material (propylene).
2) Propane analyzer-controller and reflux rate
The propane analyzer-controller is located on an upper tray and is the main control for
holding the composition of the overhead product stable. This controller is completely
analogous to an upper tray temperature controller in a conventional column like the
C3/C4 Splitter. The analyzer-controller is cascaded to the reflux flow controller and the
compressor suction drum level is cascaded to the net overhead flow. Changing the
set point of the propane analyzer-controller will affect the component distribution in the
column. The propane analyzer-controller should be set to meet the propane
specification for the final propylene product. Decreasing this set point will increase
reflux resulting in less propane in overhead but more propylene will be lost out the
bottom. Conversely, increasing this set point will allow more propane in the overhead
but less propylene will be lost out the bottom.
3) Pressure control
A slip stream of overhead vapor from the compressor is sent to the C3 Splitter Trim
Condenser where it is condensed and returned to the Compressor Suction Drum. The
flow through the condenser is varied to control pressure in the Compressor Suction
Drum and thus the pressure in the C3 Splitter.
When the propylene content in the feed to C3 Splitter has increased and/or the feed
rate to the column at a given propylene content, overall amount of propylene (and
propane which is removed from bottoms) required to be removed from the system
increases. If this is not removed system pressure would start to increase.
The HPC pressure controller (PIC) then increases the Set Point to the flow controllers
to condense out and remove more propylene as liquids and return to the HPC suction
drum. The increase in HPC suction drum with on specification purity will cause more
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product to be drawn out of the system via the product flow controller. This satisfies the
material balance to reset the system pressure.
On the other hand if the system pressure dropped (either due to reduced feed rate or
decreased propylene content in feed), the PIC would decrease the Set Point on the
flow to condenser mentioned above to permit accumulation of material within the
system allowing increasing and resetting the system pressure.
The system pressure can also increase at constant feed rate and feed quality to C3
Splitter system if the temperature of the condensed liquid products issuing from trim
condensers is not properly controlled. Increase in temperature of condensed liquids
would tend to increase the vapor pressure of the liquids accumulated in the HPC
suction drum thereby increasing the C3 Splitter system pressure. In this case the
operation of the trim condensers must be adjusted.
The system pressure can also increase if there is accumulation of non-condensable

in system which can interfere with condensing transfer coefficient in the condensers.
Even 1% non-condensable accumulation for example nitrogen can bring down the
heat transfer coefficient by as much as 33%. The solution in this case is to vent non-
condensable from the C3 Splitter vent located on HPC suction line.
4) HPC spillback flow
A spill back controller is provided which opens a bypass around the compressor if
suction flow drops too low. This is set above the minimum design flow for the
compressor to avoid surge.
5) Bottoms level controller
The bottoms product flow controller is set to cascade from the level controller on the
column bottom. It may not be practical to cascade the bottoms product flow from the
bottom level if the export rate is small relative to the capacity of the column bottom. In
this case, manually set the export rate in order to maintain a reasonably steady
bottoms level.
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7.3.4 PROPYLENE DRIERS
The propylene flows upward through the two molecular sieve driers in series. Dry
propylene then flows to the Propylene Treaters and then to intermediate storage on
back pressure control.
Periodically, the lead dryer will be removed from service for regeneration then returned
to service in the lag position. The driers must be routinely regenerated to ensure a dry
propylene product. Initially, the driers should be regenerated one after another – “back
to back” regeneration. The initial adsorption time should be 24 hours, and the
regeneration time 20-24 hour. As experience is gained and based on moisture
analysis result it will be possible to reduce the frequency of drier regenerations.
Typically adsorption time will vary between one and seven days. Please see Section
XIII-A for a more detailed discussion of drier regeneration.
The moisture content of the lead dryer effluent is measured by an on-stream analyzer.
In the event the moisture content exceeds 1 wt-ppm the lead drier should immediately
be regenerated and returned to service regardless of normal regeneration schedule.
When a drier needs to be regenerated, a slip stream of dried propylene is vaporized

and superheated for use as the regenerant. Hot regenerant flows downward through
the off-line dryer, carrying water to the Regenerant Cooler and then to the Regenerant
Surge Drum where the water is collected and sent to the Water Degassing Drum. The
spent regenerant is recycled to join the Propylene Drier feed from the C3 Splitter
overhead. The regeneration sequence can be automated for ease of operation. Refer
to Figure IV-4.
7.3.5 PROPYLENE TREATERS
Propylene from the Propylene Driers can still contain COS, arsine, phosphine and any
other metals present which must be removed to meet propylene product specifications.
The dry propylene flows upward through the treater(s) in series. The dried and treated
propylene then flows to intermediate storage on back pressure control.
Similar to the driers, the lead COS treater needs to be periodically removed from
service for regeneration and then returned to service in the lag position. The treaters
must be routinely regenerated to ensure a low metals and low COS in propylene
product. Initially, the treaters should be regenerated soon after bringing them on-line
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to ensure smooth regeneration and on-spec product. Regeneration cycle will be

determined based on individual Unit design. Usually the treaters need to be
regenerated at least once a month. The regeneration time varies between 48 and 60
hours. Please see Section XIII-B for a more detailed discussion of treater regeneration
steps.
When a treater needs to be regenerated, a stream of nitrogen is heated for use as the
regenerant. Hot regenerant flows downward through the off-line treater, carrying
contaminants to the relief header. After the regeneration is complete, the nitrogen is
vented from the treater to the relief header, and the treater is inventoried with
propylene and brought on line. Regeneration is not as frequent as for the propylene
driers. Regeneration process takes a longer time due to lower heat capacity of nitrogen.
The metals accumulated at the adsorbent cannot be removed during regeneration.
Refer to Figure IV-5.
The amount of arsine and phosphine in the propylene product cannot be easily
measured by the refinery laboratory. If the propylene metals content must be analyzed
off site, it may not be possible to reduce the frequency of the treater regenerations.
The spent treater should be immediately taken off-line and regenerated if the COS
content at the outlet is greater than 20 ppb.
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FIGURE VI-1 C3/C4 SPLITTER
FIGURE VI-2
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DEETHANIZER
FIGURE VI-3 C3 SPLITTER

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FIGURE VI-4 PROPYLENE DRIERS

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FIGURE VI-5 PROPYLENE TREATERS

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7.4 TROUBLESHOOTING
7.4.1 PRODUCT PURITY
Especially when producing Polymer Grade propylene, product purity is the highest
priority. It is essential to obtain a compositional breakdown of the impurities to
determine the source of the contamination. The contamination could be due to the
operation of the Columns or the operation of the propylene Driers and Treaters. The
major sources are listed below.
7.4.1.1 Propane
If there is too much propane in the propylene then the C3 Splitter operation should be
adjusted. Increase the reflux to wash the C3 material back down the column. Monitor
the product analyzer and once the reading is satisfactory, take a sample of the
propylene product to confirm the composition and that the changes have been
successful. How you increase the reflux will depend on the control scheme for
individual installations.
7.4.1.2 Light Ends (C2 and lighter)
Deethanizer operation must be poor if the propylene is contaminated with light ends.
Increase the reboiler rate. Check the composition of the deethanizer bottoms to
confirm if the change has been successful. The response will be faster here rather
than waiting for the change to pass through the inventory in the C3 Splitter.
7.4.1.3 Heavy Material (C4‘s)
C4 material in the propane is indicative of drawing too much material overhead on the
C3/C4 Splitter. C4‘s do not go overhead in the C3 Splitter.
The split in the C3/C4 Splitter must be rectified. It is most likely that the column is being
reboiled too hard and heavy materials are being pulled up the column and cannot be
completely removed from the overhead product by reflux. In small increments, reduce
the rate of heating medium to the reboilers and re-test the overhead product for
composition.
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7.4.2 NON-CONDENSIBLES
7.4.2.1 C3/C4 Splitter (DF-21401)
This is a very common problem at startup as the columns may have been blanketed
with Nitrogen and/or fuel gas. The C3/C4 Splitter is designed as a totally condensable
system and the pressure control on the overhead receiver will not work if there are
non-condensibles in the circuit. This will be indicated by an increase in pressure in the
Overhead Receiver which will allow the tower and drum pressures to equalize and
there will be no driving force for the vapor to exit the column.
Open the safety valve bypass to flare or if possible, vent back to the HP Separator on
the FCC Unit to remove the non-condensibles. If there is insufficient stripping in the
Gas Concentration Unit, light ends (C2-) will enter the column with the LPG and cause
a similar problem. If this appears to be the problem, check the Gas Con operation.
7.4.2.2 C3 Splitter (DF-21402)
Non-condensibles will tend to accumulate in the overhead circuit of the C3 Splitter,

raising the suction pressure of the compressor and reducing its capacity to compress
propylene to produce reflux for the column. This will reduce product purity and
destabilize the tower operation. These non- condensibles should be vented from all
high points until the operation stabilizes. Check the Deethanizer operation to ensure
there are no fresh non- condensibles entering the system.
7.4.3 PRODUCT IMPURITIES
7.4.3.1 Performance of the Driers
If the moisture in the propylene is off-spec, check the regeneration schedule of the
Dries. If the time or conditions of regeneration are not in accordance with UOP
guidelines the residual moisture in the adsorbent bed will reduce the Drier adsorption
time and can potentially lead to the water breakthrough.
7.4.3.2 Performance of the Treaters
If lab analysis indicated the breakthrough of COS, consider increasing the frequency
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of regenerations or review the regeneration conditions. If contamination is caused by

arsine or phosphine species, the adsorbent needs to be replaced.
For both Driers and Treaters: If the flow rate of material across the adsorbent is too
high, that is the liquid hourly space velocity (LHSV) is too high, the mass transfer will
be incomplete and the contaminant material could pass through the driers and/or the
treater and into the product.
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7.5.1 PROPYLENE DRIER REGENERATION
A fully automated regeneration control system can be supplied by UOP or separate

vendor. In this case there will be a control system manual provided that should be
referred to as well when operating the Driers and Treaters. The below procedure
outlines the sequence and details of all steps required to regenerate the Drier and
Treater.
Refer to the sketches in the below procedure that are marked up as follows:
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STEP 1 End Of Drier A Adsorption Stage
Drier A is operating in the lead position. Drier A is at the end of the adsorption stage
and is going to be taken off-line now for regeneration.
NOTE: Both COS Treaters should be in adsorption stage throughout the entire
process of Drier regeneration.
1. A small flow of regenerant through the vaporizer, superheater, cooler and back
to the Regenerant Surge Drum can be established prior the start of
regeneration. This can be done as shown in the sketch below
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STEP 2 Isolate Drier A

1. Open valve 16B.
2. Line up moisture probe AE to Drier B. Then close valve 16A.
3. Close valve 2B, and then open valves 1B and 3B.
4. Close valves 1A, 3A, 4A, 6A and then open bleeder valves 2A and 5A. Drier A
is now off-line:
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STEP 3 Stop Regenerant Flow
1. If the regenerant flow was on, stop regenerant flow FIC-1 at this stage in
manual. Close valves 18 and 19.
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STEP 4 Depressure Drier A
1. Close valve 12A, and open valves 10A and 11A
NOTE: Check the status of the regenerant pumps. The spent regenerant
pumps should now be started on the spillback operation, if it was not yet
done earlier.
2. Open valve 49 to line up Drier A depressurization path to the regenerant surge

drum (see sketch below)
3. Once the depressurization is complete there should be no pressure deferential
observed on PDT-1.
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STEP 5 Line Up Regenerant Path
1. Close valve 14A, and open valves 13A and 15A

2. Close valve 52, and open valve 50 and 51.
3. Open valve 21
4. Open valve 19.
5. Close valve 49.
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STEP 6 Start Regenerant Flow
1. Gradually open the valve FV-1 to start the flow of regenerant to the vaporizer.
Slowly raise the flow rate to design level and switch the flow controller to the
automatic mode.
2. Check the following:

• No sudden increase in the vaporizer outlet temperature. The temperate
should be below 55°C (131 °F)
• Level in the vaporizer remains high (over 60%) at all times.
• There are no large fluctuations in the regenerant flow to the Drier.
Rectify any issues prior to continuation.
STEP 7 Heat Up
1. Slowly open the steam pressure control valve to achieve the design steam
pressure at the vaporizer.
2. The propylene regenerant in the vaporizer will begin to vaporize and the level
will drop.
3. The regenerant superheater can be started up when:
a. At least 30 minutes have passed since the vaporizer level had dropped
below low level switch point and remained low. If the level in the
vaporizer is not low at all times, consider increasing the steam pressure
setpoint.
b. The difference between the regenerant superheater inlet and outlet
temperatures does not exceed 10°C (50°F) for over 5 minute period.
Severe damage of the electric heater bundle and polymerization may
result if the liquid propylene is left inside the heater during the start-up.
4. Turn the superheater on. Ramp the outlet temperature slowly to 235 °C (455°F)
over the 3 to 4 hour period with the rate of 70°C (158°F) per hour maximum.
The superheater outlet target temperature can be usually adjusted between
220 and 300°C (430 to 570°F) based on the regeneration requirements.
5. Hot Soak the Drier Sieve
• The Hot Soak begins when the Drier outlet temperature TT-2 reaches
at least 220°C (430°F) dependent on the superheater outlet
temperature target.
• Once the Drier outlet temperature is stabilized, 4-hour Soak time
should be held. The Soak time can be increased or reduced based on
the regeneration requirements.
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STEP 8 Cooldown
1. Start reducing the output to the superheater to lower the outlet temperature.
The superheater can be shut down once the outlet temperature reaches 70°C
(158 °F).
2. Continue cool-down the Drier with vapor until the outlet temperature TT-2 is
less than 120°C (250°F) and the difference between the Drier outlet and
superheater outlet temperatures is less 40°C (104°F).
3. Open valves 18 and 20.
4. Close valves 19 and 21. The regenerant is now lined up in the up flow direction.
5. Close the steam to vaporizer. The level in the vaporizer should start rising
quickly.
6. Cool the drier until the target Drier outlet temperature is reached. The outlet
temperature should reach 45 to 55°C (113-131°F) when the cooldown is
completed. The difference between the Drier outlet temperature and the
Superheater outlet temperature should not exceed 5°C (41°F) at the end of the
cooldown step.
Note: For those Units that have propylene Treaters with metal oxide based
adsorbent downstream the Driers, it is critical to ensure the cooldown to 50 °C
(122°F) or below is completed. Propylene stream sent to downstream treaters
must not exceed temperatures which could result in reduction of the CuO to the
elemental copper inside the adsorbent bed.
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STEP 9 Stop Regenerant Flow
1. Decrease the regenerant flow rate with FIC-1 and stop the regenerant flow.
2. Close valves 13A, 15A, 10A, 11A, 50, 51, 18, 20. Open bleeder valves 14A,
12A, and 52.
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STEP 10 Pressure Up Drier A
1. Close bleeder valve 8A. Open valves 7A and 9A to pressurize Drier A.

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STEP 11 Line Up Drier A in Lag Position
1. Close bleeder valve 5B. Open crossover valves 4B and 5B.

2. Close valves 9B and 7B. Open bleeder valve 8B.
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7.5.2 PROPYLENE COS TREATER TEGENERATION
Note: Purging or regeneration of the adsorbent should be done using

nitrogen. The nitrogen composition should be analyzed and confirmed to meet
the following specifications:
Nitrogen Analysis by Volume
Nitrogen 99.5% min.

Carbon Monoxide 20 ppm max.
Carbon Dioxide 20 ppm max.
Other Carbon Compounds 5 ppm max.
Chlorine 1 ppm max.
Water 5 ppm max.
Hydrogen 20 ppm max.
Oxygen 20 ppm max.
Noble Gases Remainder
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STEP 1 End of Treater A Adsorption Stage
Treater A is operating in the lead position. Treater A is at the end of the adsorption
stage and is going to be taken off- line now for regeneration.
NOTE: Both Propylene Driers should be in adsorption stage throughout the

entire process of the COS Treater regeneration cycle.
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STEP 2 Isolate Treater A
1. Close bleeder valve 25B, and then open valves 24B, 26B.
2. Close valves 26A, 24A, 29A, 27A, and then open bleeder valves 25A and 28A.
3. Confirm valves 18, 19, 20, 21 are closed. Confirm FIC-1 is closed in manual.
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STEP 3 Depressure Treater A
1. Confirm the regenerant pumps are running.

2. Close valve 35A, and then open valves 34A and 36A.
3. Open valve 43.
4. Depressure Treater until PDT-2 is low.
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STEP 4 Line Up Regenerant Path
1. Close valve 38A and then open valves 37A and 39A.
2. Open valve at the outlet of the Superheater (if any);
3. Close valve 52 and then open valves 50 and 51.
4. Open valve 42, and then close valve 43.
5. Verify that PIC-1 is closed, and then open valve 23 to line the steam to
vaporizer.
6. Check that regenerant pumps are running.
7. Start regenerant flow to Treater A using FIC-1. Once the design regenerant
flow rate is reached place FIC-1 in automatic.
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STEP 5 Displacement Stage
1. Slowly open the steam pressure control valve to achieve the design steam
pressure at the vaporizer.
2. The liquid propylene in the vaporizer will begin to vaporize and the level will
drop.
3. The regenerant superheater can be started up after when:
a. At least 30 minutes have passed since the vaporizer level had dropped
below to low level switchpoint and remained low. If the level in the
vaporizer is not low at all times, consider increasing the steam pressure
setpoint.
b. The difference between the regenerant superheater inlet and outlet
temperatures does not exceed 10°C (50°F) for over 5 minute period.
Severe damage of the electric heater bundle and polymerization may
result if the liquid propylene is left inside the heater during the start-up.
4. Turn the superheater on. Ramp the outlet temperature slowly to the target
displacement temperature (minimum 70°C (158 °F)). The target superheater
outlet temperature controller output must be limited to 10-15% maximum at
this stage.
5. The displacement is considered completed when the Treater A outlet
temperature increased to no more than 15 °C below the superheater outlet
temperature.
STEP 6 End of Displacement Stage
1. Gradually reduce the output to electric heater and turn the heater off.
2. Decrease and then stop the steam flow to the vaporizer using PIC-1. Close
valve 23.
3. Decrease and then stop the propylene regenerant flow to the vaporizer using
FIC-1.
4. Close valves 50, and 51. Open bleeder valve 52.
5. Close valve 42
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STEP 7 Up Nitrogen Flow
1. Open valve 45 to the relief header.

2. Verify the pressure indication at PT-2 is decreasing to below low pressure
switchpoint. The pressure differential at PDT-3 should also decrease below the
low differential pressure switch point.
3. Ensure that nitrogen controller FIC-2 is closed in manual. Close bleeder valve
48 and then open valves 46 and 47.
4. Open valve 44.
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STEP 8 Heat Up
1. Close valve 45.
2. Start flow of Nitrogen to COS Treater A using FIC-2. Slowly raise the nitrogen
flow rate setpoint to the design value.
3. Once the desired nitrogen flow rate is achieved start the superheater and raise
the outlet temperature to the target regeneration temperature of 150 °C (302 °F)
at 70°C (158 °F) maximum.
Note: Maximum target regeneration temperature for the propylene Treaters that
contain CuO based adsorbent must not exceed 150 °C (302 °F) to avoid the
reduction of CuO to elemental copper.
4. Hot Soak the bed:

• The Hot Soak begins when the Treater outlet temperature TT-4
reaches the target soak temperature, dependent on the superheater
outlet temperature setpoint and the system design.
• Once the Drier outlet temperature is stabilized, 4-hour Soak time
should be held. The Soak time can be increased or reduced based on
the regeneration requirements.
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STEP 9 Cooldown
1. Start reducing the output to the superheat to lower the outlet temperature at
50°C (122 °F) per hour. The superheater can be shut down once the outlet
temperature is below 70°C (158 °F).
2. Continue cool-down the Treater with nitrogen until the outlet temperature is
less than 50°C (122°F) and the difference between the Treater outlet and
superheater outlet temperatures is less 5°C (41°F).
Note: For CuO based adsorbent beds It is critical to ensure the cooldown to
50 °C (122°F) or below is completed. This is done to avoid initiation of reduction
of the CuO in the adsorbent to the elemental copper.
STEP 10 Pressure 1
1. Close valve 44.

2. Close valves 34A and 36A, and open the bleeder valve 35A.
3. Pressure up Treater A with nitrogen until the PT-2 increases above the
pressure-up stage pressure setpoint and stays high for at least 10 minutes
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STEP 11 End Nitrogen Stage

1. Close valve downstream the superheater (if any)
2. Close valves 37A and 39A, and open bleeder valve 38A.
3. Stop nitrogen flow with FIC-2. Close valve in manual at 0% output.
4. Close valves 46 and 47. Then open the bleeder valve 48.
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STEP 12 Pressure 2
1. Close bleeder valve 32A, the open main valve 33A and the pressurization
valve 31A.
2. Pressure up Treater A with propylene until the difference between the Treater
A pressure (PT-2) and Treater B pressure (PT-3) is less than 1 kg/cm2 for at
least 10 minutes.
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Step 13 Fill Treater A

1. Close valves 31A and 33A, and open the bleeder valve 32A.
2. Close the bleeder valve 28B, and then open Treater A inlet valves 27B and
29B.
3. Open Treater A vent valves 40A and 41A.
4. Continue filling Treater A with propylene until LT-2 indicates the steady level
greater than low level switch point.
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STEP 14 Line Up Treater A in Lag Position
1. Close Treater A vent valves 40A and 41A.

2. Close the bleeder valve 32A, and open the Treater outlet valves 30A and 33A.
3. Close valves 33B and 30B, and then open the bleeder valve 32B. Treater A is
now operating in the lag position.
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8. SPECIAL OPERATING CONSIDERATION

8.1 HP/LP Flare KO Drum (FA-21607, FA-21608)
Operator shall check the temperature (TI-21601, TI-21602) on the HP/LP Flare KO
Drum (FA-21607, FA-21608) below 60℃ before Flare KO Drum pumps (GA-
21604A/B, GA-21605A/B) start due to protect from the damage on the tankage.
8.2 Slop drain drum (FA-21606)

Operator shall check the temperature (TI-21603) on the slop drain drum (FA-21606)
below 60℃ before slop drain drum pumps (GA-21603A/B) start due to protect from
the damage on the tankage.

R2B-P3-206-02-A-FO-00001 - Rev.1 - Operation Philosophy - Eng

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PHASE II OF REFINERY IN DOS

PTI-Infraestructura de Desarrollo, S.A. de C.V.

Samsung Ingeniería Manzanillo, S.A. de C.V. /

“COMPLEMENTARY ENGINEERING, PROCUREMENT, CONSTRUCTION AND SUPPORT DURING

Contract No. PTI-ID-O-004-2-2020

1 27 AUG 21 ISSUE FOR CONSTRUCTION JG Jung YD Cho KH Lee

0 22 APR 2020 Issue for Cost Estimation JG Jung YD Cho KH Lee

A 27 MAR 20 ISSUE FOR REVIEW JG Jung YD Cho KH Lee

Rev. Date Description Prepared by Reviewed by Approved by

Rev DATE DESCRIPTION

A 27 MAR 20 Issue for Review

0 22 APR 2020 Issue for Cost Estimation

ISSUE FOR CONSTRUCTION

2.2.3.8 Oxygen ............................................................................... 31

3.3 PROCESS FLOW AND CONTROL ...................................................... 96

4.5.4 HYDROCARBON SKIMMING....................................................... 149

REGENERATED CAUSTIC ..................................................................... 188

6.5.9 DISULFIDE SAND FILTER UNLOADING PRECAUTIONS .......... 232

7.4.3.1 Performance of the Driers ................................................ 260

The FCC Unit is designed for;

2. RX-REGEN and MAIN COLUMN

2.1.1 PROJECT BACKGROUND

2.1.2 PROJECT SCOPE

Reactor Side (DC-21001)

Regenerator Side (DC-21002)

Main Column (DF-21101)

2.1.3 OPERATING CONDITION SUMMARY

UOP Yield Estimate 5325

2.1.4 PROCESS DESCRIPTION

2.1.5 FCC FEED STOCKS

2.1.6 FCC PRODUCTS

2.2 PROCESS VARIABLES

2.2.1 REACTOR (DC-21001)

2.2.1.1 Catalyst Management

Good management of the catalyst inventory is important to a smooth operation. Fresh

Fresh catalyst addition should be made as continuously and evenly as possible.

Equilibrium catalyst should be withdrawn as necessary when fresh catalyst addition

2.2.1.2 Catalyst/Oil Ratio

An increase in catalyst circulation at a constant reactor temperature will:

2.2.1.3 Charge Rate

2.2.1.4 Combined Feed Temperature

2.2.1.5 Reactor Pressure

2.2.1.6 Reactor Temperature

Reactor temperature is the prime control of reactor severity. An increase in reactor

2.2.1.7 Recycle Rate

CFR = 1 + recycle feed

Where, recycle = total of recycle rates

An increase in the recycle rate will:

1. Increase the catalyst circulation rate.

2.2.1.8 Lift Gas System

1. Increase the wet gas compressor loading.

2.2.1.9 Riser Steam

1. Decrease the hydrocarbon partial pressure in the riser.

2.2.1.10 Stripping Steam Rate

whenever there is a process change which results in an increase in the catalyst

1. An increase in the raw oil charge rate.

2.2.2 REGENERATOR (DC-21002)

2.2.2.1 Air Distribution

2.2.2.2 Catalyst Condition

Regenerator operation is not significantly affected by normal changes in catalyst

2.2.2.3 Coke Combustion

Total combustion may be initiated by using a promoted catalyst or a separate catalyst

2.2.2.4 Combustion Air Rate