S. NO.
1.0
2.0
DESCRIPTION
PAGE NO.
General
Introduction
1.1
Glosssary
1.2
Plant Description
Design Basis
2.1
2.2Process Description
2.3Equipment Description
2.4
Process Principles
2.5
Simplified Flow Diagram
2.6
Material Balance
2.7
Unit Layout Plan
2.8
Feed and Product Specification
2.9
Utility Description
2.10
Utility condition and requirement
3.0
4.0
5.0
Interconnectivity
Precommissioning Activities
Normal Start-Up
Process Variable
6.0
7.0
Normal Shutdown.
Emergency Shutdown Procedure
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8.0
9.0
10.0
11.0
12.0
13.0
14.0
15.0
16.0
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CHAPTER1
GENERAL
1.1 INTRODUCTION
Petroleum distillates normally contain small amount of mercaptans
(organic sulfur compounds) which impart obnoxious odour to the
product.
The LPG feed from FCC and Delayed Coker may contain some
mercaptans, but most of them are formed during cracking reactions.
Mercaptans are also formed when sulfur compounds decompose or H 2S
and olefins react. Mercaptans may be alkyl or aryl in nature.
UOP Merox process is an efficient and economical catalytic process for
the treatment of light hydrocarbon products . This process is used for
the conversion of mercaptan sulfur to another less objectionable form
of sulfur compound or remove the mercaptan sulfur from the
distillates. The UOP Minalk Unit (Minimum Alkali) is employing a
sweetening process to oxidize mercaptans to disulfides using air as the
source of oxygen. This reaction proceeds at nominal temperature in
presence of a catalyst in alkaline environment.
Merox treatment has the following objectives
1. To improve lead susceptibility of light gasolines
1. To improve the susceptibility of gasoline to oxidation inhibitors
1. To improve the odour of the products
2. To meet product specification
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1.2
GLOSSARY
azeotrope
antioxidant
barrel
BPD
caustic
C/H
disulfide
liquid.
chemical additive to inhibit oxidation reaction.
42 U.S. gallons measured at 60F
barrels per day (also BPSD)
sodium hydroxide solution
caustic/hydrocarbon volume ratio
class of sulfur compounds characterized by a
sulfur-to-sulfur bond and relatively low volatility
EP
extraction
GC or GLC
gph
gpm
gum
hydroperoxide
IBP
inhibitor
LHSV
mercaptan
or
PW
re-entry sulfur
enters
and
dissolves
into
by
the
weak
exiting
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RX
SCFH
sweetening
stability
desulfurization
quality of a fuel to remain unchanged for long
thiol
thiophenol
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CHAPTER2
2.1
PLANT DESCRIPTION
DESIGN BASIS
1.
2.
3.
1.
2.
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NITROGEN SYSTEM
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All lines are connected to headers or branch header are provided with
an isolation valve and spectacle blind. Following drains are connected
to main header.
From V 04 (2 line).
From LG022 and LT001 drain( both these combined and come in
2line)
Drain (2 line) from Caustic Storage tank , LG020 drain(3/4 line) and
LG020 drain(3/4 line) joins in a sub header (6 line) and this
subheader joins the main header.
This header is discharging into V 08 ( CAUSTIC DRAIN TANK). This tank
is provided with 2 nitrogen supply line through PCV 073, local press
indicator PG 061 and Flow Orifice FO 051. V08 is provided with pump P
05A & local PG 060 which is discharging to caustic system. P 05A
motor is on auto start from DCS MHS 021, run hours ML 021, based on
LI 031 low low level stop and high high level start facility is also
provided. V 08 is vented to LP flare through 8 line, which is provided
isolation valve (Valve up side down) and blind.
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2SSR + 2H2O
--- (1)
---- (2)
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Merox
2NaSR + 1/2 O2 + H2O -----> -------- + 2NaOH + RSSR
----(3)
catalyst
Mercaptans, react with sodium hydroxide to form sodium
mercaptide and water, which is reversible. The sodium
mercaptide is then oxidized over Merox catalyst, to form
disulfide, thus regenerating sodium hydroxide. The total
reaction is as follows;
4 RSH + O2 ------------>
2 RSSR + 2 H2O
------- (4)
CHAPTER 6
PROCESS VARIABLES
6.1
FEED
STOCK PROPERTIES:-
Mercaptan
: As the concentration of mercaptan
(RSH 90 WtPPM max) increases the ease of treating
decreases. Also the molecular structure of mercaptan
determines its ease of sweetening. Generally branched
secondary or tertiary alkyl mercaptans, do not get
sweetened as easily, as primary mercaptan.
Sweetening is defined as conversion of Mercaptan to
dilsulfide or some other form of innocuous sulfur
compound, without actually removing it.
6.2
REACTION TEMPERATURE
REACTOR PRESSURE :Sufficient pressure ( 5.7 kg/cm2) should be held on reactor to keep air in dissolved form. The pressure should
be sufficient to consume all the air used while
sweetening.
Channeling will take place through the
reactor if a separate air phase is present. Pressure drop
across reactor should be less than 0.7 Kg/cm2
6.4
AIR
INJECTION RATE
:-
6.5
6.6
CATALYST
UOP Merox 8 ( 44 m3 /reactor) is the catalyst used. It
is in solid form ready to use. The Merox catalyst is not
dispersible in caustic and this property prevents the
caustic from removing the catalyst from the charcoal
surface.
6.7
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2.2
PROCESS DESCRIPTION
Gasoline (Light Mogas and Heavy Mogas) from Main
column section and Unsaturate Gas concentration
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Be caustic storage
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RSH - S wppm
H2S wppm
Operating Conditions
Inlet pressure Kg/cm2 g
Inlet temperature C
:
:
90 ( Max.)
1 ( Max.)
:
:
7.7
38
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Product Quality
Mercaptan
5 ppm
CHAPTER 4
PRECOMMISSIONING
ACTIVITIES
Before initial start up;
Each vessel is to be inspected for proper fitting of
internals, valves, pressure gauges, dial thermometer
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4.1
4.1.1
LOADING PROCEDURE
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4.1.2 DISPERSION
OF
MEROX CATALYST
IN
AMMONIA WATER
and
Shake the Merox FB container to disperse any reagent that may have settled and pour the contents
directly into the drum upto 15 Kg, 6 bottles of 2.5 Kg
each of Merox reagent may be added to the drum at one
time. If more than 15 Kg of reagent is required the
reagent should be added in equal batches of 15 Kg each.
The recommended quantity of Merox FB reagent, is
approx 1.4 Kg/cubic meter of effective reactor charcoal
inventory which is the charcoal bed volume above the
outlet collector assembly.
Once the reagent has been
transferred to the drum, begin adding it to the circulating
Ammonia water via the Eductor ( Y 51 ).
The total reagent required should be added at a uniform
rate over a four to eight hour period.
Note :
The Ammonia water effluent from the reactor outlet
should remain colurless throughout the initial Merox
catalyst impregnation procedure and this should be
verified by periodically inspecting a sample of reactor
outlet Ammonia water for colour. Should the Ammonia
water from the reactor become intensely blue in colour,
there is reason to suspect channeling of the charcoal
bed in which case the catalyst Impregnation should be
stopped and steps undertaken to remove the bed
channeling. The channeling may be due to several
reasons one being improper distribution by the
distributor pipe due to breakarage etc.,
During subsequent catalyst reimpregnations, a blue
colour will appear in the Ammonia water coming from
the reactor outlet. This is not unusual, since the old
aged charcoal may no longer be able to absorb all of
the Merox reagent. Particularly some of the more
soluble isomers. As little as 1 PPM of Merox reagent is
sufficient to give a faint blue colour to the Ammonia
water.
The following procedure must be used to remove
channels
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4.1.3
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CHAPTER 5
NORMAL START-UP
Before the feed is taken into the unit, it is necessary
to expel air from all equipments and pipelines, as it is a
potential fire hazard.
Air elimination can be done by Nitrogen purging.
Entire system is lined up and air elimination done by Nitrogen
purging.
Merox Reactor ( R 01 )
Reactor should be N2 purged to an Oxygen content of
less than 5% by lining up N2 through Reactor vent line.
Reactor inlet , outlet valves to be closed and drain pot exit
valve (i/v u/s of LV001) to be closed..
Ensure all the drains and vents are closed.
Nitrogen Purging should be carried out by
Pressurising the reactor with N2 to approx 15-20 Psig.
Depressurising to atmospheric pressure.
Again pressurising the reactor to 15 - 20 Psig.with N2 and
again depressurising it to atmospheric pressure.
This
method of pressurization and depressurisation should be
repeated until the oxygen content is less than 5 vol%.
Reactor to be pressurised with FG by opening the feed inlet
valve of the reactor.
Now the system is ready for receiving Gasoline.
Steps undertaken operation are ;
Check with blending people ( RTF) whether the designated
tank is ready to receive the product. Then open the B/L
valves. Inform FCC of starting the treatment of Gasoline.
When Gasoline product from FCCU is confirmed to specified
properties, route Gasoline to Merox Unit.
Caustic injection pumps P01A and P21 to be started and
caustic injection to be started at the maximum rate..
Gasoline flow through the unit is lined up as follows:
Gasoline feed ---- Gasoline feed cooler S52 --- HV 015 ---Reactor
(R 01) ---Designated Tank or slop tank.
Gasoline feed ---- Gasoline feed cooler S53--- HV 017
----Reactor(R 21) ---- Designated Tank or slop tank.
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CHAPTER 7
R 01
R21
Merox reactor
Merox Reactor
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CHAPTER 8
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Steam Failure
CHAPTER 12
SPECIAL PROCEDURES
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CATALYST REIMPREGNATION
Requirements :
Catalyst reimpregnation is necessary only when hot
water washing is no longer effective in reactivating the
catalyst to provide long period of satisfactory mercaptan
oxidation. The internal between catalyst reimpregnation is a
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2.
3.
4.
5.
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3.
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CHAPTER 14
TROUBLE SHOOTING
The failure in mercaptan sweetening in the Merox inlet
can be attributed to one or more or combination of the
following;
a) Lack of caustic
b) Insufficient Air
c) Reactor channeling
d) Mechanical interference with the catalyst
e) Loss of catalytic activity
f) Emulsification and caustic entrainment.
Insufficient Air
(c)
Reactor Channelling
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completely
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CHAPTER 13
Y
Y
Y
Y
Y 21
51
22
03,23
53
(Y 03 )
:
:
1"
Water/0.2
5.27 Kg/cm2g
wt
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Inlet Temperature
Liquid handled
:
38C
Glacial Acetic Acid and
water
(3)
Air Mixer ( Y 04 )
Service
Hydrocarbon
Air Pipe Size
Tee Size
MOC
element
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Temp.
:
177 oC
Allowalbe temp. : 11 oC Variation
Desuperheater Water
Temp.
:
60 oC
Flow Rate :
0.11 m3/h
CHAPTER 10
LABORATORY REQUIREMENT
SCHEDULE
The ultimate objective of petroleum refining is to produce
product hydrocarbon streams which meet all specifications required for
their ultimate end use. To accomplish this objective, it becomes
necessary to characterize the important physical and chemical
properties of the various refinery streams utilizing specific laboratory
analytical testing procedures. Thus, satisfactory refinery operation
depends largely upon proper analytical procedures for quality control.
The sample point should be well purged to eliminate aged
material, water, dirt, etc., and assure withdrawal of sample
representative of the material in the pipe at that point in time. The
sample container must be adequate for the analysis to be obtained.
Once a proper sample has been obtained, it must be preserved
intact until analyzed. This require the preservation of its physical and
chemical changes in the sample.
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TEST METHOD
FREQUENCY
Once in a day
NAME
1 Gasoline Feed
Distillation
ASTM D 86
Hydrogen sulfide
UOP 163
Mercaptan Sulfur
UOP 163
Particulates
ASTM D 2276
Weekly
Gravity
ASTM D 1298
Daily
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Diagnostic
Drain Pot effluent
PH
Daily
Total Alkalinity
UOP 210
Daily
Gravity
ASTM D 1429
Daily
Acid oils
UOP 743
As required
Inhibited Product
Doctor Test
UOP 41
H2S
UOP 163
Mercaptan sulfur
UOP 163
Sodium
UOP 549
Distillation
1552
ASTM D 86
Lead content
Phosphorus
Benzene
ASTM D 3237
ASTM D 3231
ASTMD 3606
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Octane Number
Oxygen Content
VOC
EPA formula
Toxics Reduction
EPA formula
Nox reduction
EPA formula
Existent Gum
ASTM D 381
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Note:
CHAPTER 16
SAFETY
All the rules of safety in the refinery operation apply to the operation of
the Merox Process. All employees and persons responsible for
operation of the Merox process should be familiar with applicable
safety practices. All necessary precautions should be taken to avoid
accidents.
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Turbid solution
Colour
Water solubility
Complete
Molecular weight :
40.01
Flash point
Non flammable
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Inhalation
ulcerations.
Eyes
For protection of
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- Vinyl or neoprene
gloves
3. Eyes
4. Body
Neutralising Chemical
Disposal
Fire Extinguishment
First Aid
: In case of
Inhalation
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Skin contact
Eye contact
Ingestion
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CHAPTER 15
CHEMICAL CONSUMPTION
3.
4.
5.
6.
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CHAPTER 11
EQUIPMENT DETAILS
S.NO
TAG NO
EQPT.
DESIGN
OPERATING
ID MM COLUMN
TITLE
1
2
MV RF416 REACTOR
V01
MV RF
NO. 1
REACTOR
416 V02
NO.2
MOC
TEMP
PRESS
TEMP
PRESS
DEG C
70
KG/CM2G
18.7
DEG C
38
KG/CM2G
70
18.7
38
3100
CARBON
3100
STEEL
CARBON
STEEL
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VESSEL DETAILS
S.NO.
TAG NO
EQPT TITLE
DESIGN
OPERATING
ID
MM
TEMP
1
MV RF416-
DRAIN POT
V02
MV-RF416
INHIBITOR
V51
INJECTION
3*
MT-RF416-01 3
PRESS
TEMP
TANK
Be Caustic
70
3.5
70
254mmHg
PRESS
KG/CM2G
-450
38
600
Storage tank
* - Caustic Storage tank has got a partitioned section sized to hold
15% of Nominal tank capacity.
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6800
S.
TAG SERVICE
NO
NO
SET PR
PRESS KG/CM2G
TEMP DEG C
KG/CM2G
BASIS OF
SELECT
101A Reactor 1
17.5
NORMAL
5.6
MAX
18.7
NORM
38
MAX
70
FIRE
vent
101B Reactor 1
17.5
5.6
18.7
38
70
FIRE
36
30
36
38
70
BLOCKEDO
vent
102 CSTC Pump
18.2
18.7
38
70
UTLET
FIRE
18.2
18.7
38
70
FIRE
18.2
18.7
38
70
FIRE
18.2
18.7
38
70
FIRE
outlet
121A Reactor 2
17.5
5.6
18.7
38
70
FIRE
vent
121B Reactor 2
17.5
5.6
18.7
38
70
FIRE
36
30
36
38
70
BLOCKED
discharge
110A Gasoline
Cooler 2
outlet
110B Gasoline
Cooler 2
outlet
111A Gasoline
Cooler 3
outlet
111B Gasoline
Cooler 3
10
vent
122 Caustic inj
pump 2 dis
OUTLET
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S.
TAG SERVICE
NO
NO
11
SET PR
PRESS KG/CM2G
TEMP DEG C
BASIS OF
KG/CM2G
NORMAL MAX
NORMAL MAX
SELECT
151A Kero 1
24.6
14
24.6
38
70
BLOCKED
Caustic inj.
12
OUTLET
Pump A
151B Kero 1
24.6
14
24.6
38
70
BLOCKED
Caustic inj.
13
OUTLET
Pump B
152 Kero 2
24.6
14
24.6
38
70
BLOCKED
Caustic inj.
OUTLET
14
Pump
153 Air mixer out
15
to Reactor 1
154 Air mixer out
17.9
5.7
17.9
38
5.7
38
70
BLOCKED
70
OUTLET
BLOCKED
to Reactor 2
OUTLET
HEAT EXCHANGERS
S.NO TAG
NO
SIDE
SER
SURFACE
HEAT
MO
VICE
AREA
DUTY
TEMP DEG C
PRESS
KG/CM
M2/SHELL
MMK
1
S51
S53
S54
SHELL Gasoline
TUBE
CW
SHELL Gasoline
TUBE
CW
SHELL Hot Water
CAL/HR
2.43
CS
CS
5.04
CS
CS
0.82
CS
I/L
112
32
102
32
93
38
49
38
49
54
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IGN
140
120
130
120
120
8.16
3.5
9.0
3.5
4.7
wash
TUBE
effuluent
CW
CS
32
49
120
3.5
CENTRIFUGAL PUMPS
S.NO
TAG
SERVICE
SUC. PR
NO
MAX
1
RATED
KG/CM2G
P51A/B Ammoniate
1.05
1.05
PRESS
CAPACITY
KG/CM2G
M3/HR
FF
6.3
30
PO
RATED
HYD
30
3.5
d water
PROPORTIONATING PUMPS :
S.N TAG NO
SERVICE
SUCTION PR
CAPACITY L/HR
TYPE
KG/CM2G
3 oBe
P01,P21,
P31,P41
Caustic
P02,P22, Merox Plus
KG/CM2G
0.07
DIS PR
7.37
0.74
Norm
MAX
19.8 DIAPHR
RATE
28.62
AGM
DIAPHR
28.62
1.5
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P32,P42
P52,P53
3 Be
0.75
0.07
1356
136
678
Caustic
4
P03,P23,
UOP No.5
AGM
DIAPHR
13.3
AGM
0.07
6400
640
1600
6.75
P33,P43
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