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MEROX OPERATING MANUAL

INDEX

S. No. DESCRIPTION Page No.


1 INTRODUCTION
2 MEROX PROCESS DESCRIPTION
 MEROX PROCESS EQUIPMENT
 PRETREATMENT
 EXTRACTION SECTION
 SWEETENING
 POST TREATMENT
 MEROX CATALYSTS
3 U-21 ATF /SK MEROX
 UNIT CAPACITY
 FEED SPECIFICATIONS
 PRODUCT SPECIFICATIONS
 TYPE OF CATALYST USED
 PROCESS DESCRIPTION
 DETAILED DESCRIPTION OF P&ID
 PRE-COMMISSIONING OPERATION
 STARTUP PROCEDURE
 REACTOR BED WATER WASHING AND RE-
IMPREGNATION
 SHUTDOWN PROCEDURE
 EMERGENCIES
 OPERATING VARIABLES
 CHEMICALS AND CATALYSTS
 MODIFICATIONS
4 U-22 STRAIGHT RUN LPG MEROX
 UNIT CAPACITY
 FEED SPECIFICATIONS
 PRODUCT SPECIFICATIONS
 PROCESS DESCRIPTION
 DETAILED DESCRIPTION OF P&ID
 PRE-COMMISSIONING OPERATION
 STARTUP PROCEDURE
 SHUTDOWN PROCEDURE
 EMERGENCIES
 OPERATING VARIABLES
 CHEMICALS AND CATALYSTS
 MODIFICATIONS

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S. No. DESCRIPTION Page No.
5 U-23 VBN MEROX
 UNIT CAPACITY
 FEED SPECIFICATIONS
 PRODUCT SPECIFICATIONS
 TYPE OF CATALYST USED
 PROCESS DESCRIPTION
 DETAILED DESCRIPTION OF P&ID
 PRE-COMMISSIONING OPERATION
 STARTUP PROCEDURE
 REACTOR BED WATER WASHING AND RE-
IMPREGNATION
 SHUTDOWN PROCEDURE
 EMERGENCIES
 OPERATING VARIABLES
 CHEMICALS AND CATALYSTS
6 U-24 CRACKED LPG MEROX
 UNIT CAPACITY
 FEED SPECIFICATIONS
 PRODUCT SPECIFICATIONS
 TYPE OF CATALYST USED
 PROCESS DESCRIPTION
 DETAILED DESCRIPTION OF P&ID
 PRE-COMMISSIONING OPERATION
 STARTUP PROCEDURE
 SHUTDOWN PROCEDURE
 EMERGENCIES
 OPERATING VARIABLES
 TROUBLE SHOOTING
7 U-25 CRACKED FCCG MEROX
 UNIT CAPACITY
 FEED SPECIFICATIONS
 PRODUCT SPECIFICATIONS
 PROCESS DESCRIPTION
 DETAILED DESCRIPTION OF P&ID
 PRE-COMMISSIONING OPERATION
 STARTUP PROCEDURE
 SHUTDOWN PROCEDURE
 EMERGENCIES
 OPERATING VARIABLES
 MODIFICATIONS
8 SAFETY & FIRE FIGHTING FACILITIES

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1. INTRODUCTION:

Straight-run LPG, gasoline and kerosene fractions obtained from atmospheric


distillation may contain hydrogen sulphide and mercaptans. the extent of which
mainly depends upon the type of crude processed. Similar products from
secondary processes such as FCC also contain hydrogen sulphide and
mercaptans to a greater degree compared to straight-run products. Hydrogen
sulphide is corrosive and should be remove in order to meet specifications on
corrosion rate. The specification for LPG, gasolene, Kerosene and ATF include
copper strip corrosion test which is a measure of rate of corrosion on copper
containing materials.Mercaptans are substances with obnoxious odour and,
therefore, in order to handle and store them, mercaptan level will have to be
brought down to a acceptable odour level. The specifications of above products
include 'Doctor Test' which must be negative and is generally related to the extent
of mercaptan present. Hydrogen-sulphide can be easily removed by washing with
dilute caustic solution. However, for reducing the mercaptans level many
processes are available like:

Strong alkali-wash

Copper sweetening

Doctor sweetening

Merox process

Hydrodesulphurisation

Alkali-wash is effective only if low molecular weight mercaptans are involved.


Hydrodesulphurisation is normally employed only if reduction of total sulphur level
is also required. Both investment and operating costs are higher in case of
hydrodesulphurisation. Out of other proceses available, Merox process is
considered a superior and proven process.

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2. MEROX PROCESS DESCRIPTION

The Merox process licensed by M/S Universal Oil Products Co., (UOP), USA, is for
the chemical treatment of LPG, gasolene and distillates to remove mercaptans into
disulphides. The removal of mercaptans may be either partial or full. The chemical
treatment is based on the ability of Merox catalysts to promote the oxidation of
mercaptan to disulphide using air as the source of oxygen. The overall reaction is
as follows:

2RSH + 1/2O2 -> RSSR + H2O

The oxidation is carried out in the presence of an aqueous alkaline solution such
as either sodium hydroxide or potassium hydroxide. The reaction proceeds at an
economical rate at normal rundown temperature of refinery streams.

Low molecular weight mercaptans are soluble in caustic solution and therefore
when treating LPG and light gasoline fractions, the process can be used to extract
mercaptan to the extent, they are soluble in caustic. Extraction of mercaptan
reduces the sulphur content of the treated product. Alternatively mercaptans can
be converted to disulphides without removing any sulphur from the treated stock in
which case the operation is referred to as sweetening. In the treatment of heavier
boiling fractions such as heavy naphtha and kerosene only sweetening is possible.

 MEROX PROCESS EQUIPMENT:

In order to understand the function of various Merox process equipment. the


equipment can be broadly divided into following sections :

Pretreatment for removal of hydrogen sulphide and naphthenic acids, if present.


The method varies with properties and conditions of feedstock and in some cases
may not be required.

Extraction section where required, for removal of caustic soluble mercaptans and
thus reduce sulphur in the treated product.

Sweetening for conversion of mercaptans to disulphides. For a given capacity


plant, the Merox reactor size can vary depending on the case of sweetening due to
the type of mercaptans present and also on product requirement.

Post-treatment to remove caustic haze and to control properties not affected by


Merox process. Hence post-treatment needed depends on products, utilisation and
type of contaminants present in the feedstock.

Taking each section in turn, function of each equipment can be described.

 PRETREATMENT

Petroleum fractions may contain hydrogen sulphide and stocks boiling higher than
180°C may also contain naphthenic acids. Hydrogen sulphide is not a catalyst
poison as such, but will dilute the caustic containing Merox catalyst by reacting
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with caustic. Further it blocks some of the catalyst activity sites slowing down the
normal reaction and also consumes part of the oxygen available. Hence, it is
recommended that hydrogen sulphide is removed by washing with dilute alkali
solution before the distillate is sent to reactor for treatment.

Naphthenic acids also interfere with treating operations and must be removed prior
to treatment. The reactor contains caustic and if naphthenic acids are not remove
they form sodium naphthenates which coat the catalyst and block the pores. For
removal of napthenic acids, the procedure used is to wash with dilute caustic.
Dilute caustic is used so as to avoid formation of emulsions. There could, however,
be some carry-over of haze depending on the acidity of stock treated. The haze
can easily be removed by coalescing through a sand filter.

Feedstocks, where carry-over of water from distillation units can be expected must
be passed through a coalescer for removal of suspended water prior to caustic
wash, which would otherwise dilute the caustic used for pretreatment.

 EXTRACTION SECTION

As previously stated, low molecular weight marcaptans are caustic soluble and can
easily be removed by washing with caustic in a counter current tower. Improved
extraction is favored by:

Low temperature.

High concentration of caustic.

Lower molecular wt. of mercaptans

Type of mercaptans, viz. normal mercaptans are easily extractable, tertiary


mercaptans least extractable and secondary being in between.

The mercaptan enters the caustic solution and reacts as follows:

RSH + NaOH <-> NaSR + H2O

This is being a reversible reaction the degree of completion of reaction is governed


by normal equilibrium laws.

The sodium mercaptide is readily oxidised to disulphide in the presence of Merox


catalyst as shown :

2NaSR + l/2O2 + H2O -> 2NaOH + RSSR

This is not a reversible reaction and the reaction rate is speeded up by:

Raising the temperature.

Use of excess air.

Increasing the intimacy of contact.


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Increasing the catalyst concentration.

The oxidation of mercaptides is carried out in oxidiser in the presence of merox


catalyst. The disulfides oil, which is formed, separates out from caustic as it is
insoluble in caustic. Caustic can be reused for extraction. The presence of Merox
catalyst in extraction caustic does not however, affect the amount of mercaptans
extracted. and extraction is dependent only on parameters explained earlier .

 SWEETENING

Sweetening can be defined as conversion of mercaptan sulphur present in a


hydrocarbon stream to disulphide sulphur without actually reducing sulphur content
of treated stock. The sweetening process is based on the ability of Merox catalyst
to promote the oxidation of mercaptans to disulphides using air as the source of
oxygen. The reaction is as follows:

RSH + NaOH <-> NaSR + H2O

2NaSR + l/2O2 + H2O -> 2NaOH + RSSR

As can be seen from reactions, the oxidation is carried out only in the presence of
alkali solution.

The Sweetening can be accomplished either in solid bed sweetening, where the
hydrocarbons and caustic are simultaneously controlled over a solid support
impregnated with Merox catalyst.

Liquid-liquid sweetening where hydrocarbon, air and caustic containing Merox


catalyst, air simultaneously controlled in a mixer.

Solid bed sweetening consists of a reactor, which contains a bed of activated


charcoal impregnated with Merox catalyst and kept wet with caustic solution.
Impregnation of catalyst on bed is achieved by dissolving the catalyst with
ammonia solution and pumping ammonia solution over charcoal. Air is injected
ahead of reactor and in the presence of merox catalyst the mercaptans are
oxidised to disulphides. The reactor is followed by a settler which serves as
reservoir of caustic. Caustic is intermittently circulated from the settler over the
catalyst bed to wet the charcoal.

For liquid-liquid sweetening, the most common type of mixer used is the orifice
plate mixer, which is a vessel, fitted with a series of plates with orifices. The vessel
provides adequate residence time and the orifice plates create enough turbulence
to bring about the intimate contact between hydrocarbon, caustic, catalyst and air.
The problem of accomplishing liquid-liquid sweetening is one of getting the
difficulty soluble mercaptans into the caustic phase for sufficient time to permit
their oxidation. The higher the molecular weight or the more highly branched the
mercaptan is, the more difficult it is to accomplish necessary mixing. Hence heavy
gasoline and Kerosene may have to be treated using fixed bed reactor.

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 POST TREATMENT

The product from the merox reactor will at times contain caustic haze. Post
treatment is required if the product is to go to storage, clear and bright. In most
cases provision of caustic settler and sand filter is adequate to remove caustic
haze. However, for treatment of ATF, which has to meet stringent specification
caustic must be removed by water wash after caustic settling. Water wash
removes entrained caustic as well as water soluble surfactants, Water wash is
followed by a salt filter to remove entrained water and part of the dissolved water.
This may be followed by clay filter to remove copper and water insoluble
surfactants, if present in feed.

 MEROX CATALYSTS:

There are two types of Merox catalyst, each one being used for specific service.
Catalyst FB is to be used on units equipped with solid bed sweetening reactors.
Catalyst WS is used for liquid-liquid sweetening in mixers. This is a caustic
dispersible catalyst. This is also used for oxidation of extraction caustic in
oxidisers.

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3. U-21 ATF /SK MEROX :

 UNIT CAPACITY:

The Merox Unit for treating kerosene & ATF streams from the Atmospheric
Distillation unit has been designed to feed 1.5 million metric tons per year of
kerosene while processing a 50: 50 mixture of Light Arabian: North Rumalia
crudes. The Unit shall operate for 345 stream days in a year.

 FEED SPECIFICATIONS:

The kerosene to be treated in the Merox Unit shall have substantially the following
properties:

(i) Boiling Range IBP/FBP oC 140-270 Max.

(ii) Specific gravity at 15.6°C 0.795 to 0.82

(iii) Total acidity, Mg KoH/Gm 0.02

(iv) Mercaptan Sulphur wt ppm 150

(v) Total Sulphur wt.%. 0.22

(vi) H2S wt ppm 10 max

(vii) Colour, Saybolt + 30

 PRODUCT SPECIFICATIONS:

The Product kerosene/ATF after Merox treatment shall meet the following
specifications:

(i) Appearance Visually, clear, bright and free from solid


matter and undissolved water at normal
ambient temperature.

(ii) Corrosion copper strip No 1 Maximum

(iii) Corrosion silver strip No 0 Maximum

(iv) Mercaptan sulphur wt ppm 10-20 ppm (max.)

(v) Doctor test Negative

(vi) Colour loss, saybolt 5 Maximum when feed stock is 25 min.,


provided that the feed stock comes
directly from the fractionation facility.

(vii) Thermal stability:


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(a) Filter pressure drop 25.0 maximum
in mm Hg.
(b) Tube Rating visual Less than code 3

(viii) Water separameter index 90 minimum

(ix) Acidity, mg. KOH/Gm 0.012 maximum


(a) Water Separometer 90 minimum
index (modified)
(b) WATER REACTION
Interface Rating 1.0 maximum
Volume Change 1.0 maximum

(x) Conductivity (ATF) 50-450 psm

"H2S free fresh stock charge" shall mean fresh stock charge containing no H 2S or if
the fresh stock charge contains H 2S, it shall be scrubbed out with caustic soda
solution or sodium carbonate solution in the laboratory without exposure to
oxygen.

 TYPE OF CATALYST USED:

Catalyst used for sweetening kerosene/ATF Stream in this treating unit is merox
catalyst FB which is supplied by the Universal Oil-Products Company. This catalyst
is used in the two sweetening Reactors 021 R1 A and B. The catalyst is
impregnated on activated charcoal beds in the reactors. Quantity of catalyst
required for one impregnation in the reactors is 250 Kg. of active ingredient. The
catalyst is supplied in liquid from each US gallon containing 1 kg. of active
ingredient.

 PROCESS DESCRIPTION

Pretreatment for kero/ATF consists of a coalescer and caustic prewash vessel, for
removal of suspended water and hydrogen sulphide, Naphthenic acid etc.

Sweetening is achieved in supported catalyst bed reactor. Two reactors in parallel


have been provided. Air requirement of all Merox units is supplied from a common
compressor. Also, storage tanks for receipt, dilution and storage of caustic and
storage for methanol have been provided.

Post treatment for kero/ATF consists of caustic settling. water wash to wash of any
carry-over caustic salt drier for drying and clay filters for improving colour stability
of treated product. Clay adsorbs coloured nitrogen compounds.

 DETAILED DESCRIPTION OF P&I DIAGRAM

Kerosene/ATF as obtained from distillation unit stripper under flow control is


charged to the unit charge pumps 021 P4A/B. Pretreatment for kero/ATF consists
of coalescer for removal of water and caustic prewash for removal of hydrogen
sulphide, etc. The feed goes to coalescer 021-V-9 where feed passes through
pass blanket as coalescing media to coalesce tiny water droplets into sufficiently
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big droplets which settle down in the water boot provided in the coalescer. Float
type trap is provided in the water boot to drain water. Water from boot will have to
be periodically drained to oily water sewer. Provision also exists for bypassing this
vessel and directly feeding to caustic prewash vessel.

Kero/ATF from coalescer is sent to caustic prewash vessel 021-V1 (4750 mm OD


x 9150 mm) where the feed bubbles through caustic and rises to the top of vessel
due to gravity differential between feed and caustic. The feed is charged into the
vessel through a distributor pipe mounted inside the vessel and holes drilled to a
specified pattern on the distributor pipes. There are three inlet nozzles provided on
the vessel. Normally the feed should be maintained thro' the B" nozzle. Maintain
caustic level and charge caustic when the caustic is spent as indicated by its
strength. The vessel is also provided with a wiremesh in its top portion to remove
any caustic entrainment.

The feed is then mixed with air as necessary for reaction, on flow control 021 FRC
16 in the air-mixer 021 Y2 where intimate mixing of air and feed is achieved. The
feed then passes on to two reactors operating in parallel (021 RI A&B) (4000 mm
OD x 7200 m). The reactor consists of a bed of charcoal impregnated with Merox
catalyst. Impregnation being carried out as per laid out procedures using ammonia
as an agent for impregnation. The reactor bed also may need water washing and
reimpregnation to restore activity whenever catalyst activity drops. the period
depending on the type of feed proceesed in the unit.

The feed ex reactors is passed on to the caustic settler 021 V2 (3600 mm OD x


12200 mm). In the caustic settler. required settling time is provided for separation
of any carry-over caustic. Since the unit is also designed to treat ATF, which has to
meet stringent specifications, water wash and salt drier also have been provided.
Hydrocarbon from caustic settler passes into water wash vessel 021 V3 (4750 mm
OD x 9150 mm). The water wash vessel is continuously charged with
demineralised water taken from the refinery source through a water tank 021 V7
provided with a level controller 021 LC 27 which regulates water entry into water
tank. From the water tank, water is charged into water wash vessel by pump 021
P3 A & B. Flow control is by 021 FIC 24. Water hydrocarbon interface level is
maintained by 021 LC 24. The vessel is also provided with a wire mesh in its top
section to reduce water carry-over by hydrocarbons.

After water wash, hydrocarbon stream enters the salt drier 021 V4 (5000 mm OD x
8000 mm) for removal of any last traces of water. The salt drier is filled with rock
salt and the feed is distributed at the bottom of the vessel and leaves from the top.

The final step of treatment is filtering through clay towers to remove water
insoluble contaminants. For this purpose two clay filters 021-V5 A&B (4750 mm
OD x 7500) have been provided which are operated in parallel. The hydrocarbon is
distributed on top of clay filter and collected from the bottom using collector pipe
assembly wrapped with wiremesh screens. The outlet of each clay filter is
combined into a common product run down line where flow is recorded by 021-
FRQI-55. The necessary back pressure to the unit is maintained by 021-PIC-32
which ensures constant pressure in the reactor and other vessels. The treated
product is run-down to storage.

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Feed stocks which do not call for complete treatment but which meet product
specifications after caustic pre-wash, can be diverted to storage after caustic
prewash, vessel 021-V1 using the bypass line between 021-V1 outlet and
upstream of 021-PIC-32.

For meeting the requirement of caustic for all Merox units, two caustic storage
tanks 021- T1 & 021- T2 have been provided in this unit. 021- T1 is meant for
preparing and storing 3 deg. Be caustic required for caustic , prewash vessel 021-
V1. 021- T2 is meant for 10 deg. Be caustic required for reactors and other Merox
units. This unit receives 48.8 deg Be caustic from which 3 deg. Be and 10 deg. Be
caustic solution will be I prepared. DM water is used for diluting caustic.

The air reqirement of all Merox units is met by air compressors 021-C1-A & B.
Compressed air from 021-C1-A&B is supplied to other Merox units.

 PRE-COMMISSIONING OPERATIONS:

I. CHECKING OF COMPLETION OF CONSTRUCTION WORK,


INSPECTION AND BOXING UP OF EQUIPMENT

All unit equipment and pipelines must be checked to see that they conform Strictly
to the specification of design and as per drawings. Location of vents, drains, gauge
glasses, pressure gauges, sample points etc. on equipment must be checked to
ensure that they are installed in accessible locations. Also, the internal fittings in
columns and vessels like trays, packing supports screws, distributors etc. must be
checked in position and in order.

When the equipments have been satisfactorily cleared as to their internal


installations and cleanliness of construction debris, the manholes can be boxed up.

II. PRESSURE TESTING OF EQUIPMENT AND PIPELINES :

After inspection and box-up of equipment as mentioned above the entire unit has
to be pressure tested with water to maximum allowable pressure to ensure that the
plant equipment and lines can safely with-stand operating pressures. According to
convenience, equipment are tested individually or divided into sections depending
on locations and test pressure of various equipment and pipelines. proper isolation
by blinds of equipment or section under test must be done so as not to over
pressurise connected lines and vessels of lower pressure rating. Before the
hydrostatic test is undertaken, relief valves and orifice plates must be removed
from the system and blinded off. After carrying out hydrostatic tests on unit
equipment and pipelines water must be drained out completely. In order to prevent
vacuum pulling in vessels, their top vents must be opened up before attempting to
drain water.

III. WATER FLUSHING OF THE UNIT :

On completion of pressure test of the unit, water flushing of the different systems in
the unit is carried out with all the pumps running on line to flush out all muck, scale
and other construction debris contained in the lines. Suction screens must be
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installed on each pump to protect them from damage. In the initial stages of
commissioning of the unit, it is better to install a finer (60") mesh on the normal
filter of each pump. This finer filter can be removed only 2 to 3 months of actual
run of the unit when frequency of cleaning comes down to normal. The pumps are
to be run at least for 24 hours to ensure that they are running freely and smoothly.
The discharge valves of the pumps have to be suitably throttled so as not to
overload the motors during the water flushing operations. Periodically, the pumps
have to be stopped and the debris accumulated in the suction screens to be
cleared. This operation has to continue till the suction screens remain clear
continuously at least for eight hours.

When the water flushing operation has been successfully completed, all water from
the systems has to be drained out completely, especially from the low points. Air
blow the system thoroughly to remove the traces of water from equipment and
lines.

All orifice plates should be checked for proper specifications before their
installation in place. All instruments must be checked and calibrated before the unit
start-up.

IV. SCREENING AND LOADING OF ACTIVATED CHARCOAL SALT & CLAY

Activated charcoal has to be screened properly before it is loaded in the reactors.


Screening is done with 10 to 30 mesh sieve screens. To reject fines etc. which are
formed during transportation and handling coarser than 10 mesh and fines after 30
mesh are rejected from the charcoal supply. The reactors are isolated from other
equipment and their top and side man ways are opened up. The inlet distributor
pipe assembly at top has to be suitably covered to prevent any charcoal entry into
the distributor while loading. Loading is done through a hopper and adjustable
loading sock which extends to the bottom of the reactors. As the loading
progresses, the length of the sock is adjusted so that no cone formation occurs on
the charcoal surface. Improper leveling will cause maldistribution of hydrocarbon
flow through the bed. Loading personnel must wear dust masks covering the nose
and the mouth to prevent inhalation of charcoal dust. While loading, it must be
ensured that the bottom Johnson screen collector pipe assembly is fully
submerged in charcoal by physical checking from the bottom man way. The person
going inside for checking must wear a fresh air masks. The bottom man way is
then boxed up and loading continued with the sock till the inlet distributor pipe is
230 mm from the charcoal bed. The Top surface of the bed is leveled after the dust
has settled. Here again, the person entering the reactor for leveling the bed must
wear a fresh air mask. A record of loading in the reactors has to be kept for
reference and accounting, When loading to the required height is over, the loading
hopper and sock are removed the inlet distributor covering is taken off and the top
man way boxed up properly.

V. ROCK SALT LOADING :

After inspection of salt drier internals for cleanliness and fittings, it is loaded with
rock salt up to a height of 600 mm below the top tangential line. Then the top man
way is boxed up. The surface must be leveled similar to the procedure followed for
charcoal loading.
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VI. LOADING OF CLAY IN CLAY FILTERS:

The clay filters are checked for internal fittings and are cleaned up dry, prior to
loading clay. The inlet distributor pipe has to be covered suitably to prevent clay
entering into it while loading. The recommended grade of clay of the correct mesh,
30-60, is loaded from the top of the vessels. periodically leveling the surface so
that no cone formation takes place. The loading personnel going inside the vessels
for leveling must wear dust mask. The height of loading in each reactor will be up
to 920 mm from the top tangential line. After leveling of the top surface of clay in
the filters, their distributors are uncovered and the top man ways can be boxed up.

VII. IMPREGNATION OF CHARCOAL BED IN KERO/ATF MEROX


REACTORS WITH UOP REAGENT FB.

The two reactors will be impregnated as a rule one after the other, as noted below:

Start filling 21 R 1 A with DM Water. Block off Reactor outlet lines.

Start circulation pump 21P-2 after DM water level is 1 metre below top distributor
pipe. Continue to fill DM water.

When water level rises to 1 metre above the distributor pipe, stop addition of DM
water ( Be careful, not to float charcoal out of reactor )

Continue water circulation for 2 to 3 hours

Start Ammonia gas injection after the cylinder is connected in to the circulating
water. Regulate the outlet pressure at 3.0 kg/cm2, inject approximately 150 kg of
Ammonia in about 5 to 6 hours time. (Each cylinder lasts for 2 1/2 hrs). Measure the
rate by keeping the cylinder on a weigh bridge.

Keep a steam hose playing at the gas injection pipe to prevent freezing on the line.

Circulate the Ammonia solution for about 2 to 3 hrs. keeping the pump capacity to
maximum i. e. 58 M3/hr . Sample the solution and send to lab for analysis.
Ammonia concentration should be 0.2 + or - 0.02 wt. %. Add or dilute the solution
as necessary.

Meanwhile get the catalyst dissolving drum system ready with the hoses
connected. Ordinary drum of 200 liters will solve the purpose.

After achieving the required Ammonia concentration in the circulating water. route
a slip stream from 21 P2 discharge to the catalyst drum. Fill it up to 50 to 60%.
Start gentle air blowing in the Air Sprayer.

Add 7 bottles of Merox FB after shaking. Stir the mixture to help dispersing the
catalyst if required. Make up the volume to 180 litres.

Start educting the catalyst solution by routing the slip stream through the eductor
21 G-2 from 21 P-2 discharge to suction.
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Regulate the catalyst eduction rate to 3 to 4 litres/minute.

After establishing the above rate, fill the drum from Pump discharge with a rate
equal to eduction rate. Add 1 bottle of Merox FB every 10 minutes.
After about 11/2 hrs. start checking the color of the circulating Ammonia at the pump
suction before educting point. This color should be clear or faint blue. If the color is
dark blue, it means that there is channeling in the charcoal bed In such a case the
impregnation is to be stopped and Reactor bed should be flushed with air to rectify
the bed channeling.

Add 45 bottles of Merox FB.

After the last batch of solution is educted, flush the catalyst drum several times
with Ammonia solution and educt to the Reactor .

Continue circulation for about 4 hrs.

Start transferring Ammonia solution to the second reactor R1 B by opening the


inlet block valve to top distributor when the solution level in R1 A falls below top
distributor, shut off the inlet and continue to transfer all the circulating Ammonia
solution into R1B.

When the pump loses suction shut off the pump. Block in R1A. Open hydrocarbon
outlet from R1 B and start circulation back to the inlet. Start taking DM water to fill
R1 B until the level is 1 metre above the distributor pipe.

Stop DM water flow to the Reactor, but continue the circulation. Sample the
solution and analyze for Ammonia concentration.

Inject Ammonia gas again into the circulating solution to get 0.2 + or - 0.02 wt %.

Impregnate R1 B charcoal bed similar to R1 A. (Add 45 bottles of Merox FB).

After completing the impregnation of both charcoal beds, the circulating solution
can be discarded to sewer.

Drain out all the remnant Ammonia solution from both reactors to sewer. Flush and
drain each reactor with DM water to remove residual Ammonia (keeping checking
the effluent pH).

Close the top man ways of both reactors.

Start alkalising each reactor bed with 10% caustic soda solution and then circulate
the same for 2 hrs. About 8M3 of NaOH for each reactor will be sufficient.

Now the reactors are ready for commissioning with Kero/ATF.

Requirement of Catalysts/Chemicals:

(a) Merox FB catalyst -90 Bottles.


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(b) Ammonia -5 Cylinders of 60 Kg net wt.

(c) DM water -250 M3

VIII. CHARGING OF CHEMICALS:

The caustic storage tanks 021- T1 and T2 are meant to prepare and store 3°Be
and 10°Be caustic solutions respectively in them. These two tanks take care of the
caustic requirements of all the five Merox units. 26.5°Be' caustic is received in the
unit tanks prior to unit start-up. The caustic is then diluted and the solution of
required strength prepared in each tank. 3°Be' caustic is used for pre-wash in
vessel 021-V1 while 10°Be. Caustic is used in the reactors R1A and B as well as in
other Merox Units. Solutions of required strength are prepared in the unit by
diluting with demineralised water.

 START UP PROCEDURE

As soon as Kerosene/ATF becomes available from the Atmospheric Vacuum


Distillation Unit, slowly fill up the unit vessels viz., the coalescer V9, caustic pre-
wash vessel V1, Merox Reactors R1A and R1 B. caustic settler V2, water wash
vessel V3, Salt Drier V4 and the clay filters V5A and V5B one by one. Ensure all
air from the resepctive vessels is removed by opening the top vents. before filling
them with the product kerosene/ATF. Proceed further, as follows:

Fill up 3°Be' caustic solution in the pre-wash column V-1 to the specified operating
level so that the kerosene/ATF stream bubbles through caustic solution which will
absorb all the hydrogen sulphide and naphthenic acid contaminants from the feed
stock.

In a freshly charged Merox reactor no circulation of caustic is needed in the


beginning. Hence commissioning the feed charge pumps 021-P4 A/B Kerosene is
charged through the coalescer. pre-wash column, reactors and caustic settler and
the pressure are raised in the vessels to their normal operating levels.

Setting the back pressure controller 021-PC-32 on the product rundown line, for
giving the desired pressures in the vessels, air injection to the mixer 021-Y-2 is
started at the specifed rate through flow controller FRC-16. The rate of air is
approximately 30 lbs/lb of mercaptan sulphur in the feed. The back pressure
controller PC-32 is set such that all air used for the process is kept in the
hydrocarbon solution.

Initially, the product after treatment is to be routed to the slop tank. When doctor
test is consecutively negative for 2 hours the kerosene stream may be routed to its
normal storage tanks.

Water washing the product to remove the entrained caustic has to be done.
Hence, start water-washing the product, pumping DM water into the water wash
vessel 021-V3 on flow control F1C-34 through the distributor in the vessel. A

- 15 -
steady level has to be maintained by operating the controller LC-24 which controls
the spent water effluent from V-3 bottom.

The water washed product stream is passed through the drier which removes
traces of water carried over. Finally, route the product through the clay filters 021-
V5A and B to remove water insoluble contaminants and give clarity to the product.
After passing the quality control tests which are very stringent in the case of ATF,
the product is routed to the normal storage tanks. Off-spec material when treating
ATF stream is diverted to Kerosene tanks. If the feed Kerosene contains very little
mercaptans i. e. less then 10 ppm, then the entire Merox treatment may not be
required at all. It can be directly routed to run-down by-passing the treating section.
In cases where feed contains traces of H2S. but very less mercaptans, the feed
can be routed through caustic pre-wash and then direct to product run-down by
passing reactors etc.

When the plant has been fully in operation, set the feed rate to the desired level.
Check the air injection rate for mixing before reactors is adequate and ensure
proper levels are maintained in all vessels. Pressure, as already mentioned has to
be set by the pressure controller PC-32 on the product rundown line.

 REACTOR BED WATER WASHING & REIMPREGNATION

I. WATER WASHING

Over a period of time, the catalyst impregnated on charcoal in the reactors loses
its activity. Wetting the catalyst with fresh caustic circulation also may not help in
bringing the product to specifications. At this stage, the charcoal bed has to be hot
water washed to remove the organic and soap deposits from its pores and bring
back the active surface of the catalyst, for reaction. This deposition of cold organic
material on charcoal takes place gradually and hence the water washing step can
be conveniently planned to suit the product requirements. The water used for this
washing must be free of dirt, suspended matter, hardness salts and active chlorine.
Hence, steam condensate or DM water is used for washing. Proceed as follows:

Stop air injection and hydrocarbon charge to the reactors.

Pump out all the kerosene/ATF from the bottom of the reactors under steam
pressure.

Steam out the reactors for about an hour giving steam through the beds at a rate
equal to 10 lbs per cu feet of bed, i. e. about 14 MT/hr for each reactor.

Commission the water heater 021-J1 and start giving hot water at a temp. of about
85-95°C to the reactors through the distributor pipes at a rate of 8 gallons/minute
for 100 cu. feet of charcoal i.e. about 55 M 3/hr. fill up the reactors and then drain
them to the sewer at the same rate as filling water into them.

It was experienced that while using water heater (21 J1) lot of hammering was
taking place resulting severe vibration of the lines and therefore it was difficult to
maintain the water temp, Later on BFW line connection was given d/s of DM Water

- 16 -
B/V. This does not require water heater services. BFW temp. can be controlled by
controlling the steam to deareator.

Initially, the draining effluent will be dark brown and foamy which will change colour
and eventually becomes colourless. When the water from the drain is clear and
clean, the water washing can be stopped. Stop the water flow and blowout as
much water as possible from the reactor beds with steam given to reactor top.
Keep the steam flow through the beds for another 30 minutes to remove as much
residual heavy oil as possible from the charcoal bed.

Stop steam injection and block off water heater. Introduce air into the reactors and
blow the reactors well for an hour or so that there is no water drip noticed from the
bottom drain.

Next alkalize the beds with fresh 10 deg. Be caustic solution and then return the
unit to normal working condition as discussed under "Start-up Procedure".

II. CATALYST REIMPREGNATION

This step is necessary only when hot water washing, higher feed temperatures,
stronger caustic saturation, reduced feed rates etc., do not help in mercaptan
oxidation and the product remains doctor positive. The reimpregnation interval may
vary from three months to one year depending on proper prewashing feed
mercaptan content, crude source etc.

III. REIMPREGNATION OF KEROSENE/ATF REACTORS

Hot water washing.

Acidising the reactor bed.

Impregnation

IV. HOT WATER WASHING

Isolate Reactor (21 R-1 A) from the rest of the unit. Start pumping out the
kerosene, keep reactor under positive pressure by steam.

After kerosene is pumped out, start steam flow from the water heater (21J-1) to the
Reactor (Keep the bed temp. 190 deg C. Drain out the condensate from Reactor
bottom. This is to remove the residual kerosene and heavy hydrocarbon in the
bed.

Start introducing DM Water through the water heater into Reactor. Keep the water
temp. (21 T1-15) around 90-95 deg C by introducing steam into the water heater.
When the Reactor is full, open reactor bottom to drain. Keep the drain rate close to
the hot water fill rate i.e. about 50 M3/hr.

NOTE: Instead of using water heater, BFW can directly be taken.

- 17 -
Check the drain water color. When the colour is clear, check the reactor effluent
pH.

Continue hot water washing till reactor effluent pH is down to 8,9.

Follow step 1.1 to 1.5 for another reactor (21R-1B) and 23R-1.

V. ACIDISING OF REACTOR BED:

Stop the water and steam flow. Flush out the caustic circulation system by opening
up the suction lines from the reactor bottom to the circulation pump 21 P-2 and
pump discharge to spent caustic tank.

Open the top manway of the Reactor.

Refill reactor (21 R-1A) with DM water after the reactor has been pumped out till
water level is 1 M below the distribution pipe, Block in Reactor outlet line.

Start circulation from bottom to top of the reactor. Both the kerosene outlet and the
bottom pump out of the reactor are open to the pump suction. Continue to fill DM
Water till water level is 1 M above the distributor pipe.

Inject steam occasionally to keep the circulating water temp. at 50-65°C.

Take about 0.1 M3 glacial acetic acid to the Acetic acid addition pot 21V-8.

Route a slip stream from the circulating pump discharge to the eductor 21J-2. Start
educting acetic acid to the circulating system & it should be added to the system
over a 5-10 minutes period.

After circulating acidified water for about one hour check the reactor effluent pH. If
pH is higher than 6.5, add another batch of about 0.1 M 3, This acetic acid addition
is necessary to neutralise the trace alkalinity on the bed and to provide a slight
acidic medium.

Transfer the acidified water to reactor 21 R-1B and continue the circulation in 21
R-1A, Stop circulation when the level is 1 M below the distributor pipe.

Follow step 2.6 to 2.8 for acidising the bed of 21R-1B.

Transfer the acidic solution to 23R-1 from 21 R-1B with circulation on. Stop
circulation when level is 1 M below the distributor pipe.

Keep a moderate steam flow through each reactor for 30-60 minutes.

Air purge each reactor for about 60-90 minutes.

VI. IMPREGNATION

Start filling reactor 21 R-1A with DM water. Block in reactor outlet lines.

- 18 -
Start circulation pump 21 P-2 after reactor level is 1 M below the distributor pipe,
Continue to fill DM water.

When water level rises to 1 M above the distributor. Stop water addition (Be careful
not to flood the charcoal out of the reactor).

Continue circulation for about 2-3 hours.

Start Ammonia injection after the cylinder is connected. Regulate the outlet
pressure at about 3 kg/cm2. Inject approx. 150 kg of ammonia i.e about 5-6 hours
(one cylinder in 2-21/2 hrs.) Measure the rate by weighing scale.

Put steam hose to prevent freezing of pipe due to gas expansion.

Circulate ammonia for about 2-3 hours keeping the rate at pump maximum i. e. 58
M3/hr. Sample the solution and send to lab analysis. Ammonia concentration
should be 0.2 + or - 0 02 wt.%. Add or dilute solution if necessary.

After confirmation of solution concentration, route a slip stream from 21 P-2


discharge to the catalyst drum (200 litre drum). Fill it up to 50-60%. Start gentle air
blowing in the air sprayer.

Add 7 bottles of Merox FB after shaking. Stir the mixture to help dispersing the
catalyst, if required. Make up the volume to 180 litres.

Start educting the catalyst by routing the slip stream through the eductor 21J-2
from 21 P-2 discharge to suction.

Regulate the catalyst solution rate at about 3-4 litre/min.

After establishing the eduction rate, fill the drum from pump discharge with a rate
equal to the educting rate. Add 1 bottle of Merox FB every 10 minutes.

Approx. after 11/2 hour start checking the colour at pump suction before the
educting point. The colour of the solution should be clear as a very light tint blue. If
the blue colour is observed, impregnation must be stopped & reactor bed be
'fluffed' with air to correct bed channeling.

Add 45 bottles of Merox FB.

After the last batch of solution is educted, flush the catalyst drum several times
with ammonia solution and educt it into the reactor.

Continue circulation for about 4 hours.

Start transfer ammonical solution to reactor 21 R-1 B by opening the inlet


distributor block valve. When the level in reactor 21R-1A falls below the distributor
pipe, shut off the inlet. Continue/transfer to ammonical solution into reactor 21 R-1
B.

- 19 -
When the pump loses suction, shut off the pump. Block in reactor 21 R-1A. Open
HC outlet from reactor 21R-1B and start circulation to its inlet. Start taking DM
water to fill the reactor until the level is 1 M above distributor pipe.

Stop DM water flow to the reactor but continue circulation. Sample the solution and
analyse for ammonia.

Inject ammonia to get 0.2 + or - 0.02 wt. % of ammonia in the solution.

Impregnate R1 B charcoal bed in the same as way as that of R1 A (add 45 bottles


of Merox FB).

After impregnation, ammonia solution is to be transferred to VB Naphtha reactor


(To be impregnated).

Drain out all remaining ammonia solution in both reactors. Flush and drain each
reactor with DM water to remove residual ammonia, 2 hours is adequate.

Sample the charcoal in plastic bag for each reactor at three/four points.

Close the top manways.

Start alkalizing each reactor with 15°Be' caustic, use 8.5 M 3 of caustic for each
reactor. Circulate the solution for 2 hours.

The reactors are ready for kero/ATF introduction.

REQUIREMENT OF CATALYST/CHEMICALS

- Merox FB catalyst - 90 bottles

- Ammonia cylinder - 5 cylinders of 60 kg each

- Glacial acetic acid - 200 litres (approx.)

- DM Water - 250 M3

 SHUT DOWN PROCEDURE:

For planned shut down for inpsection of equipment and maintenance work in the
unit, follow the steps given below:
Shutdown air injection to the mixer and shut off feed charge pumps P4A/4B to the
coalescer 021-V9. Shut off water wash pumps P3A/3B.

Empty out the salt-drier and clay filters into the kerosene storage tanks.

If the caustic is spent in settler 021- V2, it can be pumped out to spent caustic
system for disposal. Empty out the reactors also of the spent caustic.

Kerosene remaining in the coalescer has to be drained out.

- 20 -
When all the vessels have been emptied out of their contents, they are to be
isolated by blinds. Blind list of the unit has to be kept upto date.

Steam and water wash individual equipment and systems to make them free of
hydrocarbons, caustic etc. and safe for entry. Detailed instruction for this step will
be given at the time of actual shutdown.

Entry to the vessels should be given only after making sure that they have been
isolated properly, ventilated enough, gas tested free and safe to enter.
Recommended safety equipments must be worn by workman entering the vessels
which contained caustic etc. Dust masks and fresh air equipment must be used
when charcoal loading/unloading and levelling are done inside the reactors.

 EMERGENCIES:

Emergencies can result from equipment failure and from interruption of feed and
utilities. Operators should be thoroughly familiar with the emergency procedures
and understand the reason for each move. Nature and degree of emergency
varies from time to time and hence good judgement and discretion should be
exercised to tackle such situations.

I. ELECTRIC POWER FAILURE:

If it is a general power failure, feed to the unit will be interrupted with the failure of
the pumps. Hence a shutdown of the unit is inevitable. Shut off air injection to the
mixer immediately and block off feed to the unit. Shut off discharge valve of unit
pumps and close pressure controller at unit limits and hold system pressure. Start
up the unit as per procedure when power supply is resumed.

II. STEAM FAILURE:

Local steam failure will not affect the unit running immediately, but if AVU running is
affected by the emergency, feed to the unit might be interrupted. In such a case,
the unit will have to be shutdown and kept in a standby condition pending
resumption of feed supply from AVU.

III. INSTRUMENT AIR FAILURE:

Instrument air failure will result in all unit control valves operating in the fail-safe
position, i. e., they will all close. Close off feed to the caustic pre-wash vessel V-1.
Shutdown caustic circulation pump P1, circulation pump P2 and water injection
pump P3 and block level controllers with isolation valves. Monitor all levels. Hold
system pressure by blocking off pressure controller at unit limits.

Revert back to normal operations, starting the unit following standard procedure,
once air supply to the instruments has been resumed.

- 21 -
IV. COOLING WATER FAILURE :

A total failure will effect feed supply to the unit and pumps. Hence, unit will have to
be shutdown immediately. Isolate all the pumps after stopping them. Close the
pressure controller and hold system pressure. Maintain levels in the vessels. Start-
up the unit in the normal way, when cooling water supply becomes available and
feed from AVU is restored to the unit.

V. AIR COMPRESSOR FAILURE:

If the duration of the failure is only short, the product may not go off specification.
But the mercaptan conversion efficiency drops off rapidly and the product will have
to be slopped as soon as it goes off quality. Air injection block valve has to be
immediately shut-off to the reactors R1A and B, on air compressor failure. On
resumption of air supply, check the product quality and when it is on specification,
route it to storage tank. If both the compressors are not available for a longer
duration due to break-downs and maintenance, the Unit will have to be shut-down.

 OPERATING VARIABLES:

The caustic solution used for Merox treatment viz. In pre-wash column and in
reactors become spent eventually. Weak acids like CO2 picked up from air,
naphthenic acids and other aliphatic acids present in the feed stock make the
alkalinity of the caustic lesser and its ability to extract mercaptans will suffer.
Hence, it becomes necessary to remove part of the spent caustic and replace from
time, to time to restore its alkalinity.

The feed stock should be freed of all hydrogen sulphide by passing it through the
pre-wash column. Otherwise the oxidation reaction will be suppressed in the
reactors. It will give rise to increased caustic consumption.

Lowering hydrocarbon feed rate and caustic temperature will improve mercaptan
extraction

Naphthenic acid in feed stock may give rise to emulsion problems and hence must
be removed by prewash with 3°Be caustic solution.

Oxidation rate is increased by increasing the temperature and catalyst


concentration. About 30 cubic feet of free air is required for each pound of
mercaptan sulphur to be oxidised.

The amount of Merox Catalyst needed will be approximately one pound for 1000
gallons of 25°Be caustic solution.

Sufficient back pressure must be maintained at each extraction stage to prevent


vaporisation and caustic entrainment.

Presence of acid oils upto a limit of 8% will increase solubility of mercaptans in the
caustic.

- 22 -
- 23 -
 CHEMICALS & CATALYST

Sr Vessel Initial fill,M3 Approx. Caustic Make up / change out when Quantity Expected duration
No. level of strength required with design crude
initial fill %wt
Caustic2 9.3 30-50% 2.1 When caustic strength to 1.0% About 70% of Every 9 days
1V1 of upper initial fill (drain
LG up to bottom
LG & make up)
Caustic2 51.5 Refer 6.9 Circulate reactor caustic once a 51.5 M3 Once in 5 days
1R1A/B 10oBe days. After about 5 circ. Charge
caustic caustic. Caustic strength would
tank be around 6.2%
calibrati
on chart
Acitic - - - About 250 litres for each - About once in 4
acid reimpregnation months.
21R1A/B
Activated 171 - - - - -
charcoal
21R1A/B
Rock salt 161 (200MT) - - After every 3 months run of the - -
21V4 unit. Check the salt level and
make up accordingly
Filter clay 256 - - - - -
21V5A/B
UOP 90 bottles of 7.5 - - 90 bottles required during each - About once in 4
Catalyst litres each. impregnation months at design
FB (active throughput
21R1A/B ingredient per
litre is 0.325 kg)

- 24 -
 MODIFICATIONS :

I. ANTISTATIC DOSING FACILITY

This facility is given to maintain ATF conductivity between 50 to 450 psm (PICO
simen per meter) to meet the specification.

Antistatic Agent is stored in a small vessel (0.088 M3). Two dosing pumps, 21P-
6A/B have been provided to dose ASA to D/S of 21PIC-32 as per specification.

II. ATF REPROCESSING FACILITY

With AVU revamp, ATF production has gone high. During ATF crude processing
part of untreated ATF is sent to separate tank 404 directly from AVU B/L. this
untreated ATF stored in tank can be reprocessed in kero/ATF unit at the time when
AVU is on BH crude processing. A line is layed from tank 404 to unit 21. A pump
21P7 is given which takes suction from tank 404. Pump discharge line joins to
21P4A/B suction line with a C/V and flow transmitter namely (21FRC40). This
facility can also be used for blending BH ATF with imported ATF.

- 25 -
4. U-22 STRAIGHT RUN LPG MEROX

 UNIT CAPACITY:

The Merox Extraction Unit for straight run LPG has been designed to process
70,000 MT/year of an essentially C3/C4 mixture obtained from the stabilizer
column of the Atmospheric distillation unit. The unit shall operate for 345 stream
days in a year.

 FEED SPECIFICATIONS:

The straight-run LPG feed to the Merox unit shall have substantially the following
properties:

Vapour pressure at 65°C : 17 kg/cm2 max.

C 5's mol.% : 1.0 max.

Specific gravity at 15.6°C : 0.56

Mercaptan sulphur wt. ppm. : 900 max.

Hydrogen sulphide wt. ppm : 200 max.

 PRODUCT SPECIFICATIONS :

The straight run LPG after Merox treatment shall meet the following specifications
excepting its vapour pressure shall not exceed 17.0 kg/cm 2 at 65°C.

Total Sulphur wppm: 15 max


RSH wppm : 5 max
H2S wppm : Nil
Cu Corrosion : No worse than H2S Free feed

 PROCESS DESCRIPTION:

Amine absorber for removal of H 2S and caustic prewash vessel are provided for
pretreatment.

Treatment for SR LPG consists of only an extractor with caustic, as all mercaptans
present in feed are in the extractable range. Extraction caustic is oxidised in a
common oxidiser section.

Caustic settler has been provided for settling and separation of carry-over caustic
from extractor.

- 26 -
 DETAILED DESCRIPTION OF P&ID

LPG obtained from crude unit stabiliser overhead is charged to unit by unit charge
pumps 022P-1A/B. The feed is sent to the bottom of amine absorber 022C1 (1000
mm x 19500 mm). The column is provided with 4 sieve type trays. Regenerated
DEA from amine regenerator is received in a surge drum pumps provided in
cracked LPG merox unit. DEA from surge drum is pumped to the column top on
flow control 022 FRC5. Rich DEA from column bottom is sent to amine regenerator
located in Bitumen/Sulphur unit area via level control 022 LC 4, under column
pressure. The H2S free LPG leaves from top of 022 C1 to caustic prewash vessel
022V1 ( 1100 OD x 6100 mm ) on flow control 022 FRCQI-1. Provision for
bypassing 22C-1 in running condition is made by giving a jump over from inlet to
outlet bypassing the Amine absorber. In order to keep up the extraction efficiency
constant at lower throughputs, a recirculation stream back to crude unit stabiliser is
provided. This recirculation flow can be maintained by flow controller 022 ERC 13.

In LPG caustic prewash vessel, LPG is introduced at the bottom of the vessel
through a distributor pipe. For this purpose, three nozzles at different levels have
been provided. The vessel is provided with a wire mesh at top to remove caustic
mist. Caustic in the vessel has to be replaced when it becomes spent.

LPG is then sent to the extractor 022-C-2 (1000 OD mm x 16400 mm) where
mercaptans are extracted by caustic from caustic regenerator section. The
extractor is provided with 11 sieve type trays. Caustic is charged on flow control
022 FRC-9. Rich caustic from extractor is sent to caustic regenerator section on
level control 022 LIC-8.
LPG after extractor goes to Caustic settler 022 V2 (1000 mm OD x 4000 mm).
After caustic settling LPG is run down to storage through a back pressure
controller 022PC-12 to ensure constant back pressure in the Unit. To run-down
LPG, mercaptan is added from odorant pot 022V03 by odorant pumps 022P02 to
maintain odour specification. Caustic from settler can be drained into extractor
caustic line going for regeneration.

NOTE: Mercaptan dosing pumps have been removed for some other
services and dosing lines have been blinded as dosing is not required.

- 27 -
 PRE-COMMISSIONING OPERATIONS:

I. CHECKING COMPLETION OF CONSTRUCTION WORKS, INSPECTION


AND BOXING UP OF EQUIPMENTS

The following preliminary operations have to be carried out to ensure a successful


start-up of the unit:

Check that all mechanical works of construction have been completed, equipments
inspected, boxed up and signed off on unit check lists made for this purpose.

Scaffolding, debris, tools and other construction materials removed from the unit
area.

Make a final list of blinds which should be in position or taken out before starting
purging operations. Make sure all blinds have been installed at the proper sides of
valves and signed off in the list.

Check and ensure Fire-fighting and safety equipment is in place and in good
working condition.

Ensure all utility systems and flare release headers are in service and ready for
use.

Isolate the unit from other plants and tankages at the unit limits with block valves.

Keep the fuel gas and flare header isolated from the unit pending purging
operations.

Isolate or remove orifice blocks of all flow meters for flushing purposes.

II. WATER FLUSHING OF THE UNIT :

For water flushing of a new unit, use ordinary water.

Water flushing of the entire unit has to be done with all pumps running on line so
that all muck, scale and construction debris are washed out of all equipment and
unit pipelines. The unit can be conveniently taken in sections or individual
equipment wise and the flushing operation is carried out with temporary
connections from the Fire water header. Suction screens have to be installed on
the pumps during the flushing period to protect them from damage. They have to
be run at least for 24 hours continuously to ensure their free and smooth service.
During the flushing period, care should be taken to throttle the pump discharge
valves suitably so as not to overload the motors. The screens on the pump suction
lines have to be cleared off all debris collected periodically after stopping the
pumps. till they remain clear continuously at least for eight hours. Disconnect all
instruments lead lines and flush the leads thoroughly. Make sure that all process
lines, control valve loops are thoroughly flushed, to atmosphere to remove muck,
construction debris, etc. Better to drop each C/V and flush the assembly and
bypass also thoroughly. Then the C/V can be refixed in position. Make sure all low
- 28 -
points bleeders are clear and all columns and vessels vents and drains should be
clear.

When water flushing operation is completed, we have to pressure test the entire
unit with water as detailed below:

III. PRESSURE TEST OF EQUIPMENT & LINES :

In order to check for leaks on equipment and lines after water flushing, they are all
subjected to water pressure of about 16-20 kg/cm2 .For this purpose LPG inlet to
amine scrubber and its outlet after the pressure controller are isolated by block
valves. Rich amine and rich caustic outlets from scrubber 22C1, pre-wash vessel
22V1, extractor 22C2 must also be blocked off. Initial filling of the entire unit can be
done with Fire water for removal of air. For pressurising we have to use Boiler feed
water.

Keep running the pump out of 19 P14 A/B/C group and through the permanent
supply line take BFW to this unit and slowly pressurise the entire system to normal
operating pressure for a period of 15 to 30 minutes. If necessary one or two drains
may be kept open to have a small discharge from the pump.

During pressure test safety valve down-stream flanges may be kept wedge open
or to check tight shut-off of safety valves before their set pressure.

Tighten all leaky flanges, valves glands etc. where required. Gaskets may have to
be replaced after pressure test. Keep a record of such flange joints for subsequent
testing before cutting in of feed LPG.

After the system pressure test is successfully completed depressurise the unit, but
keep the system filled with water. Now the system is ready for taking in Fuel gas.
This is the best way of keeping air out of the unit.

LPG can be taken in to the unit from Atmospheric Unit in small quantities. LPG can
be lined up slowly to pressurise the unit to a slight positive pressure with gas. This
has to be done slowly and carefully to avoid chilling. If. however, fuel gas is
available, gas can be taken directly. LPG vapourises slowly giving positive
pressure. Now drains off the water from the entire system under gas pressure.

IV. CHARGING OF CHEMICALS:

After pressurising the unit with fuel gas, inlet valve to the scrubber 22C1 is blocked
off. Ensure that DEA inlet and outlet from 22C1 are also blocked off. Similarly,
ensure that caustic charge line to 22 V1 and its exit as well as Merox coustic inlet
to extractor 22 C2 are all shut off. The Merox regeneration system is also
pressured up with fuel gas upto the disulphide separator in cracked LPG Merox
unit and the extractor 22C2 bottom valve is blocked off. Make sure air inlet valve to
the oxidiser 024-V3 remains blocked off. Alternatively regeneration section can be
filled with caustic and vented at suitable points to remove air .

In preparation for charging chemicals into the unit, vent gas from the caustic
regeneration system till the system pressure drops to 0.5 kg/cm 2. prepare 20° Be
- 29 -
caustic solution in the storage tank provided and transfer to disulphide separator
024-V4,with a good level in 24V4, start circulation pump 024-P1A/B and establish
a level in LPG extractor 22C2. Then line up the pump 24P1 A/B for circulating
caustic to extractor 22C2, through bottom LIC to the caustic heater 024-E1,
oxidiser 024-V3 and back to disulphide separator 024-V4. Adjust the circulation on
FRC control at the stipulated rate.

From the 10° Be caustic solution tank in Kerosene Merox unit, transfer enough
material into prewash vessel 22V1 to hold sufficient level. Line up lean DEA from
sulphur Recovery Unit and establish working level in amine scrubber 22C1.
Establish DEA circulation putting into commission the level controller at bottom of
the column to control the rich amine solution returning for regeneration in the
sulphur recovery unit.

 START-UP PROCEDURE:

After the precommissioning activities have been completed and all equipment and
piping etc. are purged to remove air proceed as follows:

Establish Merox caustic circulation to top of extractor column 22C2 after


establishing a working level in disulphide separator 24V4 in cracked LPG Merox
Unit.

when normal level of caustic is obtained in 22C2, commission the bottom level
controller to regulate rich caustic flow back to disulphide separator 24V4.

Charge lean amine on flow control to the amine scrubber 22C1. Maintain level at
the bottom of 22C1 by commissioning the level controller regulating the rich amine
flow to regenerator section in ARU.

Lining up the product flow upto the rundown valve at battery limits, charge straight
run LPG to the amine scrubber by means of pumps P1A and B. Control the flow
rate from the scrubber to the caustic prewash vessel 22V1 with the FRC on line.
Route LPG to rundown passing through the extractor 22C2 and caustic settler
22V2 displacing all the fuel gas to a horton-sphere lined up at LPG receiving
station.

When operating conditions become steady, with the level controllers of 22C1 and
22C2 maintaining adequate level, adjust the flow rate of LPG to the prewash
vessel 22V1 to normal rate. Commission the recycling line of LPG back to the
stabilizer column of AVU. Use the recycle line if 22C1 operates at low throughputs.

Operate the rundown line pressure controller to maintain the desired back
pressure in the system.

Check the product after caustic settler for quality. When it is doctor negative. it can
be routed to the regular storage spheres, kept ready for the purpose.

- 30 -
Commission odorant injection to the rundown LPG after caustic settler at the
specified rate. Check the odorant injection facility is ready in all respects
beforehand. Then start the injection pump 22P2 and set dosage. as instructed.

NOTE: Odorant injection is no more in use nowadays.

Check frequently LPG for H.S after the prewash vesel1 22V1 and replace caustic
as necessary. 22V1 caustic is be replaced when caustic becomes 50% spent.

Check the regenerated caustic being charged to the extractor 22C2. For
extractable sulphur in it. This will give an idea of the efficient operation of
disulphide separator.

 SHUTDOWN PROCEDURE:

Inform all concerned of intention to shutdown the unit and proceed as follows:

Shut off DEA charge pump to the scrubber 22Cl. Shut off LPG charge pump to
22C1 immediately after this. Stop odorant injection pump 22P-02.

Stop caustic circulation through the extractor 22C2 from the disulphide separator
24V4.

Stop caustic supply to pre-wash vessel 22V1.

Empty out caustic levels from 22V1, 22C2 and 22V2 to spent caustic disposal or to
the disulphide separator 24V4 in the cracked LPG Merox unit, as instructed.

Empty out DEA level in 22C1 to its regeneration section in Bitumen/Sulphur area.

Depressure the vessels and columns slowly to the flare system, after isolation at
unit limits.

Isolate the vessels and columns by blinds and make them gas and chemicals free
by water washing repeatedly, as per special instruction that will be issued at the
time of shutdown.

Keep an upto date record of the blind list.

Entry to the vessels has to be given only after ensuring that they are absolutely
free from all gases and chemicals used in the plant. Gas test must be done before
entry permit is given. Proper ventilation inside the vessels must be ensured.
Personnel entering the vessels must wear proper protective equipment as
mentioned in the clearance permits.

- 31 -
 EMERGENCY PROCEDURE

I. POWER FAILURE:

In case of general power failure LPG supply to the unit will stop and the unit pumps
running will be interrupted. DEA solution circulation also will stop.

Block off pressure controller at unit rundown line and hold pressure in the system.

Monitor all levels.

When power supply and LPG feed are restored, put the unit back into normal
operation, following standard procedure.

II. STEAM FAILURE:

In case of general steam failure, LPG to the unit will be affected and hence unit will
have to be shut down and kept under pressure till feed supply is resumed from
AVU. If the steam failure is confined to the Merox unit only then LPG Merox section
can run without any interruption.

III. COOLING WATER FAILURE:

Failure of cooling water will affect the feed supply to the unit as well as the unit
pumps. Unit will have to be shutdown and kept standby till water supply is
restored.

IV. INSTRUMENT AIR FAILURE:

On instrument air failure, all the control valves in the unit will close. If AVU is also
affected by air failure, feed to the unit will be interrupted. Close off the pressure
controller on LPG rundown line and maintain pressure in the system. Monitor all
levels till air supply is resumed to normal. Revert to normal operation.

 OPERATING VARIABLES :

I. LPG PREWASH:

LPG is passed through amine scrubber 22C1 and caustic prewash vessel 22V1 to
remove all traces of hydrogen sulphide. The DEA solution should be kept at the
specified value of 25% by wt. The amine circulation rate also should be at the
design rate of about 800 kg/hr. Caustic concentration for prewash should be 10-
20° Be, when it becomes spent, caustic must be replaced with fresh stock.

II. LPG EXTRACTOR:

Mercaptan extractor 22C2 removes these undesirable components from LPG


stream by intimate mixing with a caustic solution containing Merox catalyst. The
caustic concentration for the circulation should be 20° Be. The catalyst
- 32 -
concentration in the caustic should be 100 ppm. Merox solution circulation rate
should be 0.17 M3/hr.

Operating pressure which is maintained by the pressure controller on the rundown


line should be about 18.0 kg/cm2 at the extractor 22C2. Reducing any of these
variables excepting the pressure will affect mercaptan extraction efficiency. Too
Iow an operating pressure favours amine and caustic entrainment in LPG stream.

III. TYPICAL OPERATING DATA AS OBSERVED IN THE NORMAL RUN OF


THE UNIT

ACTUAL-1 ACTUAL-2
LPG flow M3/hr 11.76 24
Amine flow M3/hr 0.34 0.8
Caustic flow M3/hr 0.17 Nil
Back pressure Kg/cm2 12 12.5

- 33 -
 CHEMICALS & CATALYSTS:

Vessel no Initial Approx. Caustic Make up/ Quantity Exp.to


fill M3 level of strength charge out run
initial fill % wt. when reqd. when
design
crude
Caustic 022V1 3 30-50% 6.9 Caustic About 70% of Every
of upper strength down initial fill month
LPG to 1.5% (drain upto
bottom LG
and make up)
Ethyl mercap- As required to
tan - - - maintain run-
down LPG Not in use now
odour at level
2(min)

 MODIFICATIONS:

I. Facility to route SR LPG to CR LPG unit and vice-versa.

II. Facility to route CR LPG to SR LPG Xerox (unit 22) partially.

III. After AVU revamp, SRLPG make has gone up and now SRLPG is being
treated in 24 Unit which was earlier treating CRLPG.

Now SR LPG is treated In Unit 22. Following changes in operation have


been done to achieve LPG specifications.

Caustic circulation in extractor has been stopped due to caustic, carryover 8


M3 caustic is taken in this column which is acting as another prewash. Due
to high LPG production. caustic carry over continued resulting LPG falling in
Cu corrosion test. Now BFW is being taken in this column to wash the
caustic haze carried from 22V1.

IV.
Name of the Scheme for conversion of 22C2 to amine absorber
Scheme

- 34 -
Scheme No MR/PS/300/2001/12
Scheme Apr’02
implemented on
Description of Conversion of water wash column 22C2 into Amine
Scheme absorber in cracked LPG Merox

Reason for Due to higher LPG generation of around 36-38 m3/hr,


modification load on 22C1 had increased leading to very often
amine carryover from 22C1.Water wash column if
converted into amine absorber would take part of the
LPG load and would lead result in better extraction of
H2S from LPG
Operating 1. 22C2 will now be operated as amine wash
Instructions column. LPG from FCCU would get distributed in
22C1 and 22C2.10 M3/hr of LPG flow would go to
22C2 controlled through 22FRC13.
2. 22FRC13 would be given a set-point of 10 m3/hr.
3. Amine flow through 22C2 would be maintained
through 22FRC9. This would be given a set point
of 0.7 M3/hr.
4. Amine level in 22C2 would be maintained by
22LIC 8. This would always remain on auto.
5. Amine and LPG level interface is maintained in the
lower half of the column.

- 35 -
5. U-23 VISBREAKER NAPHTHA MEROX

 UNIT CAPACITY

The Merox treating unit for sweetening the naphtha stream obtained from the
visbreaker unit has been designed to feed 65,000 MT/year of naphtha. The unit
shall operate for 330 stream days in a year.

 FEED SPECIFICATIONS

DESIGN ACTUAL

H2S wppm 10 max 70-110

Mercaptan wppm 3000 max 3000-4000

Density at 15°C 0.74 0.71-0.72

Distn. IBP 50 52

FBP 116 150

 PRODUCT SPOECIFICATIONS

Merox treated naphtha shall meet the following specifications

(i) Copper strip corrosion 1 max. ASTM


( 3 hours at 50°C ) D-130-65

(ii) Mercaptan sulphur wt ppm 5 max. UOP


163-62
(iii) Oxidation stability minutes.(after injection 390 min ASTM
of UOP No.5 copper deactivator) D-525-55

 TYPE OF CATALYST USED

Merox catalyst ws which is dispersed in caustic solution is used in the extractor


column 023-C2 of this treating unit. Merox Catalyst FB is used in the sweetening
Reactor 023-R1 of the unit. This is impregnated on activated charcoal bed in the
reactor both the catalysts are supplied by UOP. Initial charge of catalyst WS is 4.0
gal. and it is added whenever spent caustic is dumped and fresh caustic solution is
made up in the extractor column for one impregnation on the reactor bed. 7.3 gal.
of catalyst FB is used.

- 36 -
 PROCESS DESCRIPTION

Caustic prewash vessel is provided for removal of hydrogen sulphide etc.

For visbreaker naphtha, both extraction and sweetening sections are provided.
After caustic prewash naphtha goes to extraction tower where partial extraction of
mercaptans, to the extent possible are extracted. Extraction is followed by
sweetening in reactor with supported merox catalyst bed. Air requirement is met
from the common compressor .

Post treatment consists of a caustic settler, and a sand filter for removing caustic
haze. The treated product requires anti-oxidant injection, since visbreaker naphtha
is a cracked product.

 DETAILED DESCRIPTION OF P&ID

Visbreaker naphtha as obtained from Visbreaker stabiliser bottom is fed to the unit
by feed pumps 023-P1 A&B.Flow control 023-FRC-3 on discharge of pump is
cascaded with visbreaker stabiliser bottom level control. Visbreaker naphtha can
be diverted to slops, when necessary,downstream of 023-FRC-3. Caustic prewash
vessel 023-V-1 ( 1000 MM x 6100 MM ) is provided for removal of hydrogen
sulphide etc. The vessel is also provided with a stainless steel wiremesh blanket at
the top to remove any caustic entrainment. There are three inlet nozzles like in
other prewash vessels. Caustic in the vessel is to be changed out as indicated by
its strength.

The feed then goes to extractor column 023C-1 ( 1000 MM x 13300 MM ) and is
introduced at the bottom of column where counter-current contact is made with
caustic under circulation. Regenerated caustic from caustic regenerator section is
introduced at column top on flow, control 023-FRC-8. Through the extractor trays
caustic flows downwards due to its higher gravity. Caustic after extraction is sent to
caustic regeneration section by maintaining the 023-CI bottom caustic level by
023-LIC-7.

In the extractor, mercaptans are partially extracted to the extent these are soluble
in caustic. About 40-60% mercaptans are normally extracted. This will vary with the
type of feed to visbreaker and operating conditions of visbreaker .

The extracted naphtha then goes to Merox Reactor 023-R1 ( 1400 MM x 4500 MM
) for sweetening of unextracted mercaptans. The reactor consists of a solid bed of
activated charcoal impregnated with merox catalyst No.1. Oxidation air is added to
visbreaker naphtha on flow control 023-FRC-15 and mixed thorougly with feed in
the air-mixer 023 M x 1 before it goes to reactor. Uniform distribution of feed over
reactor bed is ensured by the distributor pipe assembly placed inside the reactor.
The collector assembly at the bottom is wrapped with Johnson screen to ensure
filtering of reactor bed material from the hydrocarbon stream.

From the outlet of reactor, caustic removal from visbreaker naphtha is achieved in
the caustic settler 023V2( 1100 x 4700 ). The feed to the settler is distributed by a
slotted vertical pipe.

- 37 -
The treated product from settler is sent to storage via a sand filter 023-V3 ( 1400 x
3800 ) for removal of caustic haze. The inlet distributor consists of slotted pipes
assembly. Sand is filled from half way up the vessel and supported on the packing
support provided at that level. Below the sand packing segmented baffle is
provided in front of outlet nozzle' to ensure clear hydrocarbon withdrawal from
sand filter. The treated product is sent to storage after the pressure control 023-
PC-19 which ensures constant back pressure to the unit. The sand filter is also
provided with a bypass, for use when necessary.

Visbreaker naphtha being a cracked product requires to be dozed with oxidation


inhibitors. UOP No.5 inhibitor from drums can be transferred to inhibitor melting pot
023-V6. Three inhibitor metering pumps 023P-3A, B&C are provided. 023P-3A is
for injecting inhibitor into visbreaker naphtha, 023P-3C is for injecting to FCC
gasoline and 023P-3B is a common spare. Inhibitor is added upstream of 023PC-
19 control valve which ensures constant pressure.

For circulation of reactor caustic as well as for water wash and methanol
circulation, pumps 023-P2 A&B are provided. For impregnation of catalyst, catalyst
addition pot 023-V4 and flow indicators 023FI-10 & 023FI-11 are to be used when
impregnation is carried out in line with standard impregnation procedure. For
acidifying charcoal bed during reimpregnation acetic acid addition pot 023-V5 and
eductor 023-J2 are provided.

The treated and inhibited visbreaker naphtha which is


doctor sweet shall normally be used as a motor gasoline-blending component.

 PRECOMMISSIONING OPERATIONS

I. CHECKING OF CONSTRUCTION WORK COMPLETION, INSPECTION


AND BOXING UP OF EQUIPMENT.

The following preliminary operations are to be carried out in order to ensure a


trouble free and smooth startup of the unit.

Check that all mechanical works of construction have been


completed. All equipments and lines in the unit must be hydraulically tested at
pressure depending upon design conditions so that we can be certain that they will
stand operating pressures. After the hydraulic test, equipment are finally inspected
for proper internal fittings and fixtures as well as cleanliness. Clearance are given
to box up equipment after final inspection as above. Checklists are signed off as
complete in all respects for individual equipment and pipelines.

Make a final blind list indicating which blinds are to remain in position and which
are to be taken out before starting gas-purging operations. Ensure that all blinds
have been installed at the proper sides of valves and entered in the list.

Check and ensure that fire fighting and safety equipment are readily available in
the unit in good working condition.
Ensure that all utility systems and flare release header are in service and ready for
use.

- 38 -
Ensure free movement in the unit area. Get scaffoldings, construction debris tools
and tackles etc. removed from the unit area.

Isolate the unit from other plants and storage tanks at the unit limits with block
valves/blinds for carrying out flushing and purging operations.

Isolate or remove instrument orifice blocks for flushing purposes.

II. WATER FLUSHING OF THE UNIT

In preparation for start-up of the unit, water flushing of the entire unit has to be
carried out to remove and wash out all muck, scales construction debris etc. from
equipment and lines for the purpose of water flushing, the unit can be taken up in
convenient sections as well as individual equipment-wise also. Hooking up
temporary fire water hose connections on equipment or lines, thorough flushing of
all equipment and lines are carried out.

All the unit pumps are tried out during water flushing with suitable wire mesh
screens ( preferably 100 each )fitted on to their suction spools to prevent them
from damages. The pumps have to be run at least for 24 hours continuously to
ensure their free and smooth functioning. Care has to be taken while running the
pumps not to overload their motors, during the water flushing operations Their
discharge valve have to be suitably throttled to take care of the loads on motor.
During the pumps running-in period, the suction screen will get choked up with
debris washed out into them and they will start losing suction. Immediately the
pumps are to be stopped. screens opened up, cleaned and then pumps restarted.
This cleaning operation will have to be continued till the suction screens remain
clear of all debris and muck at least for 8 hours.

On satisfactory completion of water flushing of the unit. All the water from
equipment and lines are to be drained out, opening drains and flanges at low
points. Care should be taken not to pull any vacuum in the equipment while
draining water. Then, thoroughly air blow the entire unit to remove all traces of
water remaining after water washing.

III. PRESSURE TESTING OF EQUIPMENT & PIPELINES

Subsequent to water flushing of equipment and lines in the unit, a pressure test is
carried out with water to about 10 kg/cm2 to detect leaks, if any, in the system and
repair them in the time before the actual start-up of the unit and to tighten most of
the flanges. During the test safety valve downstream flanges are opened up to
check holding of safety valves. Any safety valve which requires resetting is
removed and sent to workshop for repair.

Pressure test with water can be conveniently carried out by running the feed pump
or caustic pump and pressure up the unit by restricting the flow at the plant outlet
till the desired pressure is reached. Care has to be taken during pressure test to
isolate equipment and piping which are designed for lower pressure, like e.g.
methanol system. These can be tested separately at lower pressure.

- 39 -
After pressure test is satisfactorily completed, drain water from system at all low
point and air blow it thoroughly to remove all moisture.

IV. SCREENING AND LOADING OF CHEMICALS

ACTIVATED CHARCOAL

Activated charcoal which merox catalyst impregnation will be


screened properly before it is loaded in the reactor 23R1. Standard ASTM Sieve
Nos. 10 and 30 screens have to be used and charcoal coarser then No.10 and
fines after No.30 screen are separated out. The charcoal thus screened is loaded
in 23R1 after isolating it from other equipment. Its top and side manways are kept
open. Its inlet distributor pipe assembly has to be kept 'Covered during loading to
prevent charcoal entry into the pipe. Charcoal loading is done through a hopper
and adjustable canvass chute, which extends to the bottom of the reactor. As
loading progresses, the length of the chute is adjusted. No cone formation is to be
allowed on the charcoal surface in the reactor. Improper leveling will cause non-
uniform distribution of hydrocarbon flow through the charcoal bed.

Personnel must wear dust masks covering their noses and


mouths to prevent inhalation of charcoal dust, while loading for leveling inside the
reactor, the person entering must wear a fresh air mask. While loading, it has to be
ensured that the 'bottom Johnson screen collector Is fully submerged in the
charcoal by physical checking, from the bottom manway. The charcoal loading is
continued till the inlet distributor pipe is about 900 mm from the charcoal bed. Final
leveling is done entering the reactor top with protective equipment. Record of
quantity of charcoal loaded in the reactor is kept for reference. The loading hopper
and canvas chute are removed after loading, the cover on distributor pipe is taken
out and the top maway of the reactor is boxed up tight.

SAND

Check the internals of sand filter 23-V3 for proper


fittings and support for sand 'bed, Check also it is wiped clean from inside sand
screened to the specification of 8-16 ASTM Nos. is then loaded to a height of 1.4
meters in the filter. The surface is levelled properly and then the vessel is boxed up
finally.

V. PRESSURE TEST FOR TIGHTENESS

When all chemicals have been loaded as required and all manways, flanges, etc
boxed up the unit is ready for impregnation of catalyst on charcoal bed. Before
impregnation of catalyst, it is preferable to test the unit for tightness of flanges,
manways. etc. under air pressure. Compressed air ex 21 CI A, B can be used for
pressuring up the unit to about 10 kg/cm2' pressure.

After the unit is pressured up. check all flanges manways, etc for tightness with
soap solution. Tighten as required. When pressure test is over release the
pressure gradually in order not to disturb the bed of charcoal.

VI. IMPREGNATION OF CATALYST ON REACTOR 23-R1


- 40 -
After the reactor is filled with charcoal to the required level and boxed up proceed
to impregnate charcoal with Merox catalyst FB as detailed in the following steps.

Fill the reactor with DM water being careful not to add so much water as to float
charcoal out of reactor.To ensure this. reactor top manway can be kept open. Once
level is ensured manway can be kept in closed position without bolting to enable
inspection of bed after impregnation.

Stop D M water supply and line up reactor bottom to reach


circulation pump 23-P2 A. B and establish from bottom of bed to top of bed.

Estimate the amount of water in the system i. e. reactor, lines etc. If water is
charged from a tank, this can be estimated conveniently from tank dips. Estimate
should take into account piping, dead spaces etc. The total quantity will be about
6-7 M3.

Calculate the amount of ammonia required to raise the


concentration of water to a 0.2% wt solution of ammonia. The quantity of ammonia
required will be about 12-14 kgs.

With water in circulation, inject the desired amount of ammonia into the water
upstream of suction line to pump 23-P2 A. B. Ammonia is injeted from a cylinder
mounted on a suitable weighscale so that the quantity of ammonia injection can be
controlled. Adjust ammonia injection rate in such a way that the amount needed
will be introduced during the time it takes to pump the entire water inventory
through this system twice; with pump this would takes 3 to 4 hrs and hence adjust
ammonia injection to last this period.

When ammonia concentration is uniform in the system. fill the catalyst mix drum
with ammonia water. Add the content of 3 bottles of 2.5 gallons each of merox FB
catalyst. This contains 7.5 kg of active ingredient. Mix ammonia water and catalyst
solution thoroughly using an air sparger. In the catalyst mix drum do not exceed
80% level.

With water still circulating from the bottom of the reactor to top, educt the catalyst-
ammonia water into the system at a rate of approximately 4 liters per minute.

After emptying the mix-drum, flush it several times with Ammonia water and educt
the water into the reactor to get all of the residual catalyst into the reactor.
Continue circulation of ammonia water for one more hour after all catalyst has
been educted. Finally drain all water from the system.

The catalyst is now ready for alkalizing with a 10°Be solution of caustic. Transfer
caustic of this strength to the settler 23V2 to about 30% of its volume. Start caustic
circulation with pump 23-P2 A/B through the reactor 23-R1. Initially keeping the
drain valve open, remove all the free water till caustic appears at the drain. Close
off the drain and continue circulation at the maximum discharge rate for about two
hours. If necessary. take additional caustic from storage tank into settler 23-V2.
Stop circulation after two hours and the reactor is now ready after impregnation to
receive hydrocarbon feed for sweetening.
- 41 -
VII. CHARGING OF CHEMICALS

Caustic requirements of the unit is met from the storage facility available in the
kerosene merox section. Fresh caustic of 26.5 %Be strength is received in storage
tanks 21 TI & T2 and diluted with demineralised water to the desired strength.
10oBe caustic is charged into the prewash vessel 23-V1 till a working level is
established in 23-V1. 20°Be caustic from the disulphide separator 24-V4 of the
cracked LPG Merox Unit is charged to the extractor column 23-C1 top through a
11/2" line by the transfer pump at cracked LPG Merox Unit. This caustic drop after
extraction of mercaptans is sent back to the regeneration section on level control
from the bottom of extractor column. To begin with 20°Be caustic is transferred to
the disulphide separator from kero merox unit to establish sufficient level for
subsequent transfer to other merox sections.

 START-UP PROCEDURE

It is assumed that the merox system is fully lined up for startup. Proceed to start-up
the unit as follows :-

When visbreaker naphtha becomes available commission the charge pumps 23-
P1 A/B and slowly introduce naphtha into the prewash vessel 23-V1 and fill it up.
Let it pass through the extractor and then the reactor and caustic settler. Finally,
pass naphtha through the sand filter 23-V3 to the rundown line to storage. Vent out
all air before filling the vessels.

Commission the pressure controller 23-PC-19 to have the required back pressure
in the system.

Maintain proper levels of interface in 23-V1 and 23-C1.Commission the bottom 23-
LC7 of 23-C1.

Start air injection thro' mixer 23 MY1. Take the flow on control 23-FRC15 and set
the flow rate to the requirement (30 kgs/hr.) of mercaptan sulphur in the feed. 23
PC-19 should be set such that all air injected is in hydrocarbon solution.

In a freshly charged merox Reactor, no caustic circulation will be needed on the


initial start-up period. Hence it is enough to pass the feed through the reactor, with
air mixing as already mentioned above. When catalyst activity declines over a
period of time, resaturation with caustic circulation is resorted to.

Caustic carried over alongwith naphtha is settled in 23-V2 and drained back to the
circulating pump suction. Any traces of caustic haze still remaining is removed in
the sand filter 23-V3 and the treated naphtha is routed to storage from the sand
filter.

Commissioning the inhibitor injection facility, the metering pump 23-P3A/B is


started to inject the measured quantity of inhibitor into the naphtha stream going
out to storage. The present injection rate is 80 to 90 ppm so as to get a minimum
induction period of 360 minimum.

- 42 -
Initially, the product stream is routed to the slop tank till satisfactory results are
obtained consistently for about 2 hours. Then naphtha can be routed to the regular
storage tanks. Set the feed rate to normal consistent with other control systems
parameters.

 REACTOR BED WATER WASHING & CATALYST REIMPREGNATION

Over a period of time, catalyst in the reactor bed loses its activity and even wetting
with fresh caustic circulation does not help in restoring the activity and the product
continued to go off specifications. Then the charcoal bed has to be hot water
washed to remove the organic deposits on its pores. Washing will bring back the
activity of the catalyst for reaction again. As the loss of activity by deposits on
charcoal surface occurs gradually the water washing operation can be planned
conveniently The water used should be dust free and free from suspended matter.
hardness, salts and active chlorine. DM Water is therefore, used in our plant for
this purpose. Water washing procedure is as follows :

Stop air injection and hydrocarbon charge to the reactor 23 R1.

Pump out all naphtha from 23 R1 under steam pressure. Steam out the reactor for
about an hour.

Commission water heater 23 JI and start introducing hot water into reactor at a
temperature of 85 - 95°C at a rate of 8 gallons/minute for 100 cubic feet of
charcoal bed i. e. about 3.5 M3/hr. Fill up the reactor and drain water to sewer at
the same rate as filling.

The effluent from reactor bottom will be dark brown and foaming in the beginning.
This will change and become colourless gradually when water washing
progresses. When the drain water is clean and clear. The washing of the reactor
bed can be stopped. Then blow out as much water as possible from the reactor
with steam given to it from the top. Continue steam blowing for another half an
hour to remove from the charcoal voids as much residual heavy oil as possible.

Stop steam to reactor and block of water heater. Blanket the reactor with nitrogen
and blow it with N2 gas for an hour or so till there is no water dripping from the
bottom drain.

Next alkalize the reactor bed with 10 oBe caustic solution and then return the unit
back to normal operations, as detailed under "Start-up procedure."

I. CATALYST REIMPREGNATION

Catalyst reimpregnation step is necessary only when hot water washing, higher
feed temperature, stronger caustic reduced feed rates etc. do not help in
mercaptan oxidation and the product remains off-spec. Gap between one
reimpregnation and another will depend on proper prewashing, feed mercaptan
content, crude etc. Period may vary from three months to one year depending on
feed quality. Detailed steps for reimpregnation are as given below:

- 43 -
Follow the steps 5.1.1 to 5.1.4 given under "Reactor Bed Water washing",
excepting the steaming of reactor. Fill up the reactor with hot water. Then stop
water and steam flow to the water heater by blocking off the valves.

Line up reactor bottom drain line to caustic circulation pump 23 P2 A/B and flush
out the lines free of caustic into the spent caustic disposal system.

Close the reactor outlet valve and fill it up with hot water again. Start hot water
circulation from reactor top to bottom, regulating water temperature with steam
around 50-70°C. Keep both the drain line and reactor outlet lined up to the
circulating pump.

Take about 20 liters of glacial acetic acid in the addition pot 23-V5 and close the lid
of 23- V5. Educt the acid from 23-V5 into the circulating water with the help of the
3/4" globe valve on pump 23-P2 A/B discharge. Eductor 23-J2 takes suction from
the acetic acid addition pot 23-V5. Educt the acid to the circulating water to reactor
over a period of 5-10 minutes.

Circulate the acidified water for an hour and check its PH at the pump 23-P2 A/B
suction. If PH is more than 6.5 another 20 litres of acetic acid will have to be
educted till the circulating water PH is 6.5 or less.

Stop water circulation; introduce steam into the reactor and remove all water from
the bottom drain. Keep steam blowing for another half an hour and displace all
traces of residual oils from charcoal voids. Stop steam to reactor and blow it with
air till water drips from its drain stop.

Then follow the steps given under "Impregnation of catalyst" under 3.6. Unit can be
returned to its normal duty as soon as reimpregnation of catalyst is over.

 SHUTDOWN -PROCEDURE

For planned shutdown for inspection of equipment and maintenance work in the
unit, follow the sequence of operations given below:

Inform all concerned of intention to shutdown the unit. Shut off air injection block
valve to the mixer MX1.

Shut off naphtha charge pump 23P1A/B to the prewash vessel 23 V1.

Close off the pressure controller 23PC-19 at the battery limit. Shut off anti-oxidant
injection pump 23P3A/B to the naphtha stream before 23 PC-19.

Stop caustic circulation through the extractor 23C1 and reactor 23 R1. Pump out
caustic from 23 C1, 23 R1, 23 V2 and 23 V3 to spent caustic disposal system.

Pump out all caustic from 23 V1 bottom into the spent caustic drainage system.

Pump out hydrocarbons remaining in the vessels to the slop tank with circulation
pump 23 P2 A/B.

- 44 -
Flush out reactor 23 R1 with hot water thoroughly and drain off all water.

Isolate all individual equipment by blinds as required for maintenance. Steam and
water wash them thoroughly till they are hydrocarbons and chemicals free.

Maintain an upto date blind list of unit equipment.

Follow detailed instructions that will be given at the time of shutdown for preparing
equipment and lines gas free and for maintenance.

Entry to the vessels should be given only after ensuring complete isolation by
blinds, making gas free and free of chemicals. Also, it must be ensured that the
vessels are well ventilated and are safe to enter. Gas test must be taken before
issuing clearance for entry into a vessel Safety equipments recommended must be
worn by personnel entering vessels which previously contained caustic and other
chemicals.

 EMERGENCIES

Emergencies result out of equipment failures and from interruption of utilities.


Operating personnel must be thoroughly familiar with the emergency procedures
so that quick actions can be taken in such situations. Nature and degree of an
emergency varies from time to time. Hence, good judgement and discretion should
be exercised to tackle any emergency.

I. ELECTRIC POWER FAILURE

If it is a general failure, naphtha feed to the unit will be lost and all unit pumps will
stop. Unit will have to be immediately shutdown. blocking off air injection to mixer
MX1. Close off the pressure controller at battery limit and hold the system
pressure. Shut off the discharge valve of pumps. Hold the levels in the vessels.
Start up the unit again following standard procedure. when power supply is
restored.

II. STEAM FAILURE

Local steam failure will not effect the unit immediately If the naphtha feed supply
from visbreaker is affected then unit will have to be shutdown and kept standby till
the feed naphtha is available again.

III. INSTRUMENT AIR FAILURE

All control valves will operate to fail safe position i.e. they will close. Shut off the air
to the reactor by the block valve to the mixer MX1. Hold the pressure in the system
and monitor all levels till air supply is restored to the instruments. Start-up the unit
as per normal procedure and bring it back on stream.

IV. COOLING WATER FAILURE

A total water failure will affect feed supply to the unit as well as unit pumps. Hence.
unit will have to be shut down immediately. Stop the pumps. Block off pressure
- 45 -
Controllers and hold system pressure. Maintain all levels in unit vessels. When
cooling water becomes available, start up the unit, as per normal procedure.

For a short duration, process air failure will not affect the treated naphtha quality.
But the mercaptan conversion efficiency drops off rapidly with no air for oxidation.
Hence the product will have to be stopped as soon as it becomes doctor positive.
Shut off air injection block valve to mixer MX1 immediately on air failure.

 OPERATING VARIABLES

Caustic solutions used in prewash vessel 23 V1 and reactor 23 R1 become spent


eventually and mercaptan extraction will suffer. Hence, periodically, part of the
caustic will have to be replaced with fresh stock.

Caustic concentration in the solution for extracting lighter mercaptans in 23 C1


must be 20°Be.

Catalyst concentration in caustic should be 100 ppm.

Operating pressure should be about 8 kg/cm2 to keep the air injected dissolved in
hydrocarbon. Lower pressure results in vaporisation and caustic entrainment.

Too little air will result in incomplete oxidation of mercaptans to disulphides. About
30 cu. feet of free air is required for each lb of mercaptans sulphur to be oxidised.

Catalyst activity in the reactor bed is increased by resaturation with 10°Be caustic
circulation freshly taken and circulated through the bed. Hot water washing and
reimpregnation with catalyst are further steps to restore the activity of the catalyst.

Acid oils upto 8-12% in caustic solution will increase solubility of mercaptans in
caustic.

H2S and naphthenic acid from feed naphtha must be fully removed in the prewash
vessel 23 V1. Otherwise oxidation reaction will be suppressed in the reactor.
Naphthenic acid may give rise to emulsion problems.

I. Typical Operating Data :

DESIGN ACTUAL

Feed flow M3/hr 10.5 2.4 to 4.0

Air rate NM3/hr 7.1 3.0 to 6.0

Caustic Circulation rate M3/hr 25 2 to 2.5

Feed temperature: °C 40 30-35

- 46 -
 CHEMICALS & CATALYSTS

Sr Vessel Initial Approx. level of Caustic Make up / change out Quantity Expected duration
No. fill,M3 initial fill strength %wt when required with design crude
23V1 2.4 30-50% of 6.9 When caustic strength to About 70% of initial fill Every month
upper LG 1.5% (drain up to bottom
LG & make up)
23R1 1.5 Refer caustic 6.9 Circulate caustic once in 15 M3 Once in 45 days
tank calibration 9 days. Caustic good for
chart about 5 circulations
Ammonia 12-14 - - Some quantity required - About once in 4
23R1 kg during each months at design
reimpregnation throughput
Acetic - - - About 20 litres for each - About once in 4
acid 23R1 reimpregnation months at design
throughput
UOP No.5 About - - Rate of injection 760 - 10 drums good for
oxidation 10 cc/hr 6 months
inhibitor drums
UOP About - - Rate of injection 1000 - 3 drums good for
copper 3 CC/hr of mixture of UOP six months
deactivato drums No 5 & deactivator in the
r ratio of 1:0.32
Charcoal 6.0 - - - - -
23R1
Sand 2.2 - - - - -
23V3
Catalyst 7.5 gal - - 7.5 gal for each - About once in 4
Merox for impregnation months at design
reagent initial throughput
FB 23R1 impreg
nation

- 47 -
6. U-24 CRACKED LPG MEROX

 UNIT CAPACITY

Cracked LPG Merox unit is designed to process 1,45,000 MT/Year of LPG from
Catalystic Cracking Unit with an on stream days 345 per year.

 FEED SPECIFICATIONS

C5 + material - < 1% (Mol)


H2S - < 2100 WPPM
RSH-S - 300 WPPM (Max)

 PRODUCT SPECIFICATIONS

LPG PRODUCT:
Total sulphur - < 15 WPPM
RSH-S - < 5 WPPM
Copper Corrosion - Not worse than H2S free feed.

 TYPE OF CATALYST USED

The Merox Catalyst used in the extraction section of this unit is UOP Merox WS. It
is a replacement for the original conventional powdered Merox Reagent No.2.
Merox WS is an aqueous solution of the reagent having equivalent catalytic activity
and stability as merox Reagent No.2. Although it is not truly soluble in water, it has
got considerable dispersibility in caustic solution. It is packed in polythene bottles
with 1 kg. of active ingredient in each bottle of 3.8 litters capacity.

Catalyst is added to the circulating caustic going to regeneration section. The initial
inventory in a process unit is recommended at 100 PPM (by wt.) or approximately
1 bottle per 4 M3 of caustic soda and up to 5 times this concentration in units
treating high severity FCC gasoline.

One distinguished characteristic of this Merox Catalyst leads to a simple control of


unit operation. If mercaptans or excessive amounts of acid contaminants such as
sulfides are absent. A medium containing approximately 100 WPPM Merox
catalyst imparts a deep blue color. However should mercaptan be added, the
solution will become deep green.

In this complex state, the catalyst exhibits a considerably greater ability to remain
suspended. If the mercaptans in this green merox catalyst medium were oxidized,
the blue color would reappear This phenomenon can, be observed in the shake
test which is an extremely useful parameter in evaluating the process.

- 48 -
 PROCESS DESCRIPTION

THEORY OF MEROX TREATMENT OF CRACKED LPG:

The extraction mode of Merox Process is for the treatment of light hydrocarbons in
LPG and light naphtha streams. It is designed to reduce the total sulfur content by
extracting the mercaptan compounds in these streams. The extracted mercaptan
compounds can be effectively removed after being oxidized to disulfide oils. The
Hydrocarbon stream is contacted with caustic solution in an extractor. Extracted
mercaptans are then oxidized and separated from the caustic. Thus the Merox
process is easily described in two parts:

MERCAPTAN EXTRCTION

Mercaptans present in the LPG are readily dissolved in the caustic solution when
extracted by means of a high efficiency, counter flow extractor. As the hydrocarbon
and caustic are intimately contacted, the mercaptans combine chemically with the
sodium hydroxide molecules.

RSH + NaOH <-> NaSR + H2O

Since the reaction is reversible, the sodium mercaptide must be removed from the
caustic solution from time to time. The UOP designed counter amount extractor
provides the effective extraction of mercaptans in to the caustic solution and its
removal from cracked LPG.

MEROX CAUSTIC REGENERATION

Caustic regeneration is for the removal of sufficient mercaptides from the rich
caustic solution to allow the reuse of this caustic solution to continuously affect the
desired mercaptan removal from the hydrocarbon stream. Sodium mercaptides in
the rich caustic are readily oxidized to disulfide in the presence of oxygen and
enough Merox catalyst. Sodium hydroxide reliberated. This is represented as:

Merox
NaSR + 1/4 02 + 1/2 H2O -------> 1/2 RSSR + NaOH
Catalyst

This is an irreversible reaction.

The disulfide oil produced is essentially in soluble in the caustic solution and thus
allow it to be gravity separated from the regenerated caustic before the lean
caustic is allowed to return to the extractor.

The composite reaction is

RSH + 1/2 02 -> 1


/2 RSSR + H2O

The composite reaction does not consume caustic, if only the mercaptans are
extracted. However the other extractable compounds such as H 2S, C02, COs do
not allow full recovery of caustic. Pretreatment of hydrocarbon stream becomes
- 49 -
necessary to remove maximum amount of H 2S. This is accomplished by Amine
absorption followed by washing with dilute caustic of 7% by wt.

Post treatment is normally for the removal of entrained caustic solution due to its
corrosive nature to protect down stream process equipment and to meet product
specification.

 DETAILED DESCRIPTION OF P & I D

The cracked LPG from FCC gas concentration stabilizer overhead is received in
amine scrubber 24C1 (14000 mm x 19500) having 11 absorption trays

Lean amine from Amine Regeneration unit located in Sulphur plant area after
regeneration is received in surge drums 024 V7 (900 mm x 3100 mm). The entry of
amine into surge drum is controlled by 024 LC 28 to maintain level in the vessel.
The drum is maintained under pressure by blanketing with sweet fuel gas as
available from fuel gas amine absorption unit The pressure controller 024 PIC 31 is
a split range controller with two control valves one on the fuel gas line and one on
the flare line. Amine from surge drum is pumped to 024 C1 by pumps 024 P2 A & B
on flow control 024 FRC-5. The pump also delivers amine to amine absorber of
unit 022 for SR LPG. There is also a minimum from bypass line from discharge to
suction of the amine pumps for use when pumped out quantity is less.

In 024 C1 amine enters the top of the column and LPG is introduced at the bottom.
Counter-current absorption takes place as LPG rises up through the perforated
trays provided in the column. Rich amine from column bottom is sent to Amine
Regeneration unit under column pressure. The flow of rich amine is controlled to
maintain column bottom level by 024 LlC 4. LPG from top of 024 C1 goes to
caustic prewash vessel 024 V1 on flow control 024 FRC-1, which is cascaded to
FCC gas conc. stabilizer overhead vessel level control. In order to keep good
extraction efficiency at low throughputs or to have good control on flow in case flow
of LPG is unsteady, part of LPG from extractor can be circulated back to FCC
stabilizer overhead vessel, using 024 FRC 27 for overall LPG flow control.

LPG to caustic prewash vessel (1600 x 6100) can be distributed into the vessel
using one of the three distributors provided. Normally the one at the bottom is
used. Caustic in the vessel is changed out whenever caustic strength comes down
below specified level. The vessel is provided with an SS wire mesh blanket to
minimize caustic mist carryover.

LPG after removal of hydrogen sulfide in absorber and prewash vessel goes to
extraction column 024 C2 (1400 x 13300) for extraction of mercaptans. The
extractor is fitted with 7 trays of perforated tray type. Regenerated caustic from
caustic regeneration section enters the top of column on flow control 024 FRC-9.
Extraction of mercaptans takes place in the column and extracted LPG from top of
column is sent to caustic settler 024 V2 (1400 x 5600). Rich caustic from bottom of
extractor goes to caustic regeneration section. The flow of rich caustic is controlled
to maintain bottom level by 024 LlC 8.

LPG is introduced into the caustic settler through a slotted vertical pipe distributor.
The caustic settling down in settler can also be diverted to caustic regeneration
- 50 -
section. LPG from top of settler is sent to storage. Back pressure controller 024 PC
11 on run-down line maintains sufficient and constant back pressure in the unit.
Injection of ethyl mercaptan to maintain odor level is also done on the run-down
line. Mercaptan storage and pumping facility is common for straight run LPG and
cracked LPG.

The extractor caustic from straight run LPG, visbreaker naphtha and cracked LPG
are combined together for caustic regeneration. The combined caustic goes to
caustic heater 024 E1 where caustic temperature can be increased by about 10°C
or so to favor caustic regeneration reactions. The heating is with steam and to
avoid caustic embrittlement it may be necessary to operate with a minimum back
pressure on steam-side to ensure lower condensation temperature.

Air required for oxidation is introduced into caustic at the outlet of heater. 024 FRC-
13, 024 FRC-14, & 025 FRC-15 have been provided on the airline to regulate air
flows to suit caustic flows from three merox units. A special spring loaded check
valve mounted in the airline ensures proper mixing of air and caustic going to
oxidize. Merox catalyst as necessary is injected into caustic going to oxidizer at a
point upstream of heater. For preparation of catalyst slurry & injection, catalyst
addition pot 024 V6 (450 x 900) and necessary hose connections are provided.

Caustic-air mixture enters oxidizer 024 V3 (700 x 7000) at the bottom through a
slotted horizontal pipe distributor. The vessel is filled with 1 1/2" carbon rasching
rings upto the top cover. The bed of carbon rasching rings packing provides
sufficient contact surface necessary for oxidation of mercaptides in caustic. The
caustic containing mercaptides, which are oxidized to disulfides, leaves at the top
of vessel and goes to disulfide separator.

The disulfides in caustic after oxidizer are insoluble in caustic and hence separate
out when caustic is given enough settling time. The disulfide separator vessel 024
V4 (1600 x 6500 & 450 x 1800) is provided in line to separate out disulfide oil and
to safely vent out unreacted air which will separate in the vessel. This is a
horizontal vessel provided with anthracite packing as coalescing medium to
separate out disulfide oil. A small cylindrical vessel known as 'skim pot' packed
with steel rasching rings in its top portion is mounted on one side of the vessel.
The separated air will contain traces of disulfide vapor mercaptans, and traces of
hydrocarbon. Because of its composition, a possibility exists for destructive internal
combustion. The steel rasching ring packing ensures relatively short residence
time for the vapors and also prevents propagation of flame should it ever occur.
Besides the steel rings reduce the possibility of ignition occurring due to static
discharge.

The regenerated caustic enters the skim pot of separator at a point just below the
ring packing, through a horizontal slotted pipe distributor. Caustic level is
maintained in the skim pot by 024 LIC 25 by controlling the flow rate of incoming
caustic to regeneration section which is achieved by controlling either one of
extractor caustic streams; coming from SR LPG, Cracked LPG or VB naphtha
meroxes.

Caustic flows across the vessel through the anthracite packing to effect separation
of disulfide from caustic. The anthracite packing in the form of fine powder is held
- 51 -
between two support rings which hold wiremesh screens supported on grating
bars. For searing of the supporting grids, nylon ropes are used. Disulfide oil which
separates out while passing through the anthracite packing floats on top of caustic
From time to time as indicated by level disulfide oil shall be pumped out to slop
tanks. From the disulfide outlet nozzle there is a line connecting to skim pot vent
off any air, which does not separate in the skim pot. While pumping out disulfide oil
from vessel. It is advisable to check the level of caustic in skim pot and ensure that
the level is sufficiently below the vent line joining from disulfide outlet line.
Otherwise there is a chance of draining out caustic alongwith disulfide oil.

The Caustic from the bottom of the separator is circulated back to extractor column
by caustic circulating pumps 024 P1 A&B. The caustic streams to extractor
columns are all under flow control in the respective merox units. As regulating one
of the rich caustic streams from extractors controls the caustic level in separator,
that particular extractor will be without any bottom level control. Hence the
extractor level should be watched carefully and if necessary maintain a slightly
higher level to take care of surges in hydrocarbon level which would upset the
column bottom level. If the caustic flow to oxidizer tends to fluctuate due to
hydrocarbon surges. It is advisable to commission the hydrocarbon recycle stream
at the outlet of extractors in order to hold steady flow to extractor and variable flow
on to recycle streams. The recycling stream facility is provided in SR LPG and
cracked LPG merox extractors. If necessary fresh caustic can be added into the
system.

The air, etc. from the top of separator is safely disposed off either by venting it at a
high point or by diverting into a nearby firebox. The back pressure controller 024
PC 24 on the vent line ensures necessary & constant back pressure in the caustic
regeneration section. There is an oxygen analyzer 024 AR 22 placed on the line to
monitor continuously the composition of gas and should it fall in the combustible
range, This will activate the solenoid valve trip system placed on the air-line to
oxidizer. Thus cutting-off air supply to oxidizer.

The vent gas can be diluted with fuel gas to reduce oxygen concentration. 024 FI
26 on fuel gas line indicates locally the flow rate of gas which can be adjusted
depending on the vent gas composition. This will support combustion in the
firebox. The vent gas is lined up to 019 F1 fire box. Two flame arrestors are
provided upstream of fire box entry. One of them shall be lined up.

If a firebox is not available, the gas can be vented to atmosphere via vent tank 024
V5 (450 x 1800) exhausting the material at a high point. Fuel gas addition is to be
stopped in this case. The vent tank is filled with steel rasching rings in its top
portion on a suitable support. Any condensate collection in the vessel is drained to
sewer automatially by gooseneck drain piping.

LIST OF PACKINGS

(1) Oxidizer -11/2" carbon Rasching rings


(7000 mm height)

(2) 24-V-4 Dome -1" steel Rasching rings

- 52 -
24-V-4 Horizontal portion -4 to 8 mesh anthracite coal

(3) Vent tank -1" steel Rasching rings

NOTE :- The packing details should be checked with U.O.P original project
books.

 PRECOMMISSIONING OPERATION

Checking completion of construction works, inspection and boxing of equipment.

The following preliminary checks should be carried out to ensure a successful


startup of the unit.

Check that all the mechanical works of construction have been completed as per
project book.

Check the entire erection of the unit, equipment and lines and compare with the
Process and Instrumentation diagrams and any discrepancies should be pointed
out and corrected.

Scaffolding, debris, tools and other unnecessary construction material should be


removed from unit areas.

Make a final list of blinds which should be in position or taken out before starting
purging operations. Make sure all blinds have been installed at the proper sides of
valves and signed off in the list.

Check and ensure Fire-fighting and safety equipment is in place and in good
working condition.

Ensure all utility systems and flare release header is in service and ready for use.

Isolate the unit from other plants and tanks at the unit limits with block valves.

Keep the fuel gas and flare header isolated from the unit pending purging
operations.

Isolate or remove orifice blocks of all flow meters for flushing purposes.

WATER FLUSHING OF THE UNIT :

Water flushing of the unit is meant for thorough cleaning of equipment internals,
and entire piping; so that all muck, scale and construction debris are removed
completely. Water supply can be taken by temporary hoses from the fire hydrant
systems. The unit can be conveniently divided into small sections and the flushing
operations are to be carried out. All pumps suction screens should be fitted with
fine mesh wires during the flushing operations to protect the pumps' internals. The
following precautions are very important during flushing out period.

- 53 -
Isolate all instruments, disconnect the lead lines and flush thoroughly each lead
line.

Drop control valves and flush through the inlet, outlet and bypass lines thoroughly.

Disconnect pumps' suction flanges; keep tin sheet to prevent water getting in to
the pumps; open suction strainer flanges, pull out the strainer and flush each
suction line to outside thoroughly. Then only we can make up the pumps suction
flanges and run the pumps for further effective flushing.

While running the pumps; the fine strainer gets choked quite often; and needs
frequent cleaning. These fine strainers can be totally removed only after cleaning
frequency comes down to once in 8 to 10 hours.

While flushing the entire system, make sure that all low point bleeders are proved
clean.

PRESSURE TEST OF EQUIPMENT AND LINES

The cracked LPG unit contains two sections. The LPG treatment section operates
at 15 to 16 kg/cm2 pressure, whereas the Regeneration section operates at 5
kg/cm2. The pressure testing of these two sections should be done independently
to check for leak and for rectifying the same.

NOTE :-Caustic regeneration being common to SR LPG and VB Naphtha Merox


Units in addition to CR LPG Merox Unit, it depends upon which Merox Unit is being
commissioned first. Naturally the first unit to be commissioned will be SR LPG; so
also all the precommissioning and commissioning activities of caustic.

Regeneration Section will have to be done at this time.

The procedural details are noted below:

PRESSURE TEST OF MEROX TREATMENT SECTION

The high-pressure section consists of Amine Absorber, caustic prewash, Merox


extractor, caustic settler and the various connected high-pressure lines and
pumps.

This system will be pressure tested after complete isolation from Regeneration
Section with water supply from 19-P-14A/B/C. For this purpose LPG inlet to Amine
absorber and its outlet after pressure controller are isolated by block valves. Rich
amine and rich caustic outlets from 24-C-1, prewash vessel V1 and 24C-2 must
also be blocked off.

Initial filling of the Merox treatment section can be done from fire hydrant water
with a temporary hose connection. Fill up the entire system and equipment with
water and displace air completely. Pressurizing the system can then be done by
taking Boiler feed water supply from 19-P-14A/B/C. Slowly raise the system
pressure up to 18 to 20 kg/cm2. Check for leaks in the entire high-pressure section
and rectify the same. One or two bleeders can be kept slightly open so that Boiler
- 54 -
feed water pump will have some positive discharge. The amine surge drum test
pressure will be around 1 to 1.5 kg/cm2 only. So this needs pressure testing
separately from high-pressure section and can be done independently by initially
filling the vessel with water and then pressuring with hydraulic pumping. After
pressure test fuel gas backing in to this vessel should be done by separate hose
connection.

After successful completion of pressure testing, depressurize the section to around


0.2 kg/cm2 water pressure.

Now pullout all blinds in the unit as preparatory step for unit startup and keep
system isolated by block valves only.

Cut in fuel gas or take small quantity of LPG into the system and let it evaporate.
Slowly the system water should be totally drained out under fuel gas pressure.

PRESSURE TEST OF REGENERATION SECTION

This section can be pressure tested with service air up to 5 kg/cm2. The caustic
heater, oxidizer, disulfide separator and connecting lines and equipment are
subjected to this pressure. With soap solution check for leaks and rectify the same.
Then depressurize the regeneration section to atmosphere. In this section there is
no need to displace air because later on air will be injected in to this system as per
process needs.

CHARGING OF CHEMICALS

After pressuring up the unit with fuel gas, and total draining of water inlet valve to
the scrubber C1 is blocked off. Ensure that DEA inlet and outlet from C1 are also
blocked off. Similarly, ensure that caustic charge line to V1 and its exit as well as
Merox caustic inlet to extractor C2 are all shut off.

Prepare 20°Be caustic solution in the storage tank provided and transfer to
disulfide separator 024-V4. With a good level in V4, start circulation pump 024-P-
1A/B and establish a level in LPG extractor 24-C-2. Then line up the pump P1A/B
for circulating caustic to extractor C2, through bottom LIC to the caustic heater
024-E1. Oxidizer 024-V3 and back to disulfide separator 024-V4. Adjust the
circulation on FRC control at the stipulated rate.

From the 10oBe caustic solution tank in kerosene Merox unit. transfer enough
material into prewash vessel V1 to hold sufficient level. Line up lean DEA from
sulfur Recovery Unit to Amine surge drum 24-V7. Entry of Amine in to V7 is
controlled by 24-LC-28 to maintain a level in the vessel. The drum is maintained
under pressure by blanketing with sweet fuel gas available from fuel gas amine
absorption unit. The pressure controller 24-PIC-31 is a split range controller with 2
control valves one on fuel gas line and one on the flare line. Establish working
level in amine scrubber c1, using 24-P-2A/B and 24-FRC-5. Establish DEA
circulation putting into commission the level controller at bottom of the column to
control the rich amine solution returning for regeneration in the sulfur recovery unit.

ADDITION OF MEROX CATALYST: W. S.


- 55 -
While commissioning a fresh unit. there is no need to add catalyst in the beginning.
We can add catalyst only when the circulating caustic becomes partly spent after
absorption of Mercaptans from the LPG. But we will describe the steps for adding
the catalyst here.

Calculate the approximate quantity amount of caustic circulating from regeneration


to extractor 24-C-2 and back. This will be equal to 16 to 18 KL.

The rate of addition of catalyst is approximately a bottle for every 4 M 3 of


circulating caustic.

Prepare slurry of catalyst in caustic taken in a bucket. Then transfer the slurry to
the make-up pot. Mix the slurry thoroughly in the pot by using Air sparger provided.

Transfer the solution under air pressure in to the circulating caustic.

It is desirable to add the total catalyst in small lots of 1 to 2 bottles at a time to


ensure uniform distribution over the entire circulating caustic.

Same principle for catalyst addition will be followed whenever part of the caustic is
replaced with Fresh caustic to ensure minimum catalyst presence and activity in
the caustic.

 START-UP PROCEDURE

After the pre-commissioning activities have been completed the unit will be
commissioned as per standard procedure noted below:

Charge circulating caustic solution to top of extractor column C2 after establishing


a working level in disulphide separator V4 in cracked LPG Merox Unit.

When normal level of caustic is obtained in C2. commission the bottom level
controller to regulate rich caustic flow back to disulphide separator V4.

Charge lean amine in flow control to the amine scrubber C1. Maintain level at the
bottom of C1 by commissioning the level controller regulating the rich amine flow
to regenerator section in SRU.

NORMAL START-UP PROCEDURE

At this stage all the chemicals are charged to the unit and the unit ready for taking
in hydrocarbon.

Line up cracked LPG flow from battery limit to Amine scrubber -> Caustic prewash
(bottom two distributors) -> Extractor-> Caustic settler -> Back pressure controller.
Commission the controller and set it at 15 kg/cm 2.

Open battery limit valve and direct LPG flow to Amine scrubber. Be prepared to
draw more DEA from Amine regeneration unit as the Amine scrubber trays are
being washed with Amine. Set the Amine flow FRC.
- 56 -
Fill the scrubber, prewash and extractor vessels with LPG, As extractor is being
filled, caustic solution level in the regeneration section may be made to fill up the
circulating caustic inventory. Make sure there is always some caustic level in the
extractor. LPG should never be allowed to enter regeneration section.

Once the unit is filled with LPG and is at the operating pressure (of to 22 kg/cm2 at
the inlet of the unit), check LPG flow rate and verify all the gauge glasses.

Commission steam to caustic heater to maintain the inlet temperature to oxidiser at


45° C. Start air injection.

Commission back pressure controller 24-PC- 24 and set it at 3.5 kg/cm2. Send
waste air to vent tank 24V-5.

Commission oxygen analyser. Once oxygen concentration in the vent air is below
12% (by vol), start fuel gas. Set FRQI-26 at a flow rate such that oxygen content
after dilution should fall below 5% ( by vol ). Send air/fuel gas mixture to the
highest disposal point in to the atmosphere.

As disulphide/caustic inter phase appears in the horizontal body of the disulphide


separator, open disulphide oil disposal line to 24-P-3. The formation of disulphide
oil will be very little and will be discharged to slop oil tank. The pumping is
expected to be intermittent. Make sure that some disulphide oil is seen in the sight
glass of disulphide separator. Do not pump out caustic also.

Check the product after caustic settler for quality. When it is doctor negative, it can
be routed to the regular storage bullets, kept ready for the purpose.

Commission odorant injection to the rundown LPG after caustic settler at the
specified rate. Check the odorant injection facility is ready in all respects
beforehand. Then start the Injection pump P-O2 and set the dosage as instructed.

Check frequently LPG for H2S after the prewash vessel V1 and replace cautic as
necessary. Check the acid oil content of the caustic solution once in a week. If it is
more then 8-12% then some caustic from V-1 will have to be replaced.

Check the regenerated caustic being charged to the extractor C2. This will give an
idea of the efficient operation of disulphide separator .

 SHUTDOWN PROCEDURE :

Inform all concerned of intention to shutdown the unit and proceed as follows :

Shut off DEA charge pump to the scrubber C1. Shut off LPG charge pump to C1
immediately after this. Stop odorant injection pump PO 2.

Stop caustic circulation through the extractor C2 from the disulphide separator V4.

Stop caustic supply to pre-wash vessel V1.

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Empty out caustic levels from V1 C2 and V2 to spent caustic disposal or to the
disulphide separator V4 as instructed.

Empty out DEA level in C1 to its regeneration section in SRU.

Depressure the vessels and columns slowly to the flare system, after isolation at
unit limits.

Isolate the vessel and column by blinds and make them gas and chemicals free by
steaming and water washing repeatedly, as per special instructions that will be
issued at the time of shutdown.

Keep an upto date record of the blind list.

Entry to the vessels has to be given only after ensuring that they are absolutely
free from all gases and chemicals used in the plant. Gas test must be done before
entry permit is given. Proper ventilation inside the vessels must be ensured.
Personnel entering the vessels must wear proper protective equipment as
mentioned in the clearance permits.

 EMERGENCIES:

I. POWER FAILURE

In case of general power failure LPG supply to the unit will stop and the unit pumps
running will be interrupted. DEA solution circulation also will stop.

Block of pressure controller at unit rundown line and hold pressure in the system.

Monitor all levels.

When power supply and LPG feed are restored, put the unit back into normal
operation, following standard procedure.

II. STEAM FAILURE

In case of general steam failure, LPG supply to the unit will be affected and hence
unit will have to be shut down and kept under pressure till feed supply is resumed
from FCC.

III. COOLING WATER FAILURE

Failure of cooling water will affect the feed supply to the unit as well as the unit
pumps. Unit will have to be shutdown and kept standby till water supply is
restored.

IV. INSTRUMENT AIR FAILURE

On instrument air failure, all the control valves in the unit will close. If FCC is also
affected by air failure. feed to the unit will be interrupted. Close off the pressure

- 58 -
controller on LPG rundown line and maintain pressure in the system. Monitor all
levels till air supply is resumed to normal. Revert back to normal operation.

 OPERATING VARIABLES

1. Amine concentration -25% by wt. in water.

2. Lean DEA temperature -As low as possible.

3. DEA circulation rate -10 M3/Hr.

4. LPG feed temperature -35 to 40°C.

5. Inlet pressure -22 kg/cm2.

6. Caustic prewash -10°Be (Caustic conc.)

Change out the caustic at 50% spent or H2S break through.

7. Merox causitic concentration -18 to 20°Be.

8. Caustic circulation rate -4 M3/Hr.

9. Extractor inlet pressure -20 kg/cm2.

10. Oxidizer inlet temperature -45 to 48°C.

Air injection to maintain

1.78 NM3/kg of Mercaptan Sulphur (initially)


45 to 60 seconds, shake test.
8 to 12 vol % of oxygen vent gas.

Lean Merox Caustic

Caustic concentration -18 to 20° Be.


50 to 100 wt ppm of NaSR

If this figure is exceeding dump out around 6 M 3 of 24-V-4 caustic to ETP , take
fresh caustic into the system and add Merox Reagent No.2 as required.

LPG PREWASH

LPG is passed through amine scrubber C1 and caustic prewash vessel V1 to


remove all traces of hydrogen sulphide. The DEA solution should be kept at the
specified value of 20%wt. The amine circulation rate also should be at the design
rate of 10 m3/hr. Caustic concentration for prewsh should be 10°Be when it
becomes spent. caustic must be replaced with fresh stock.

LPG EXTRACTOR
- 59 -
Mercaptan extractor C2 removes these undesirable components from LPG stream
by intimate mixing with a caustic solution containing Merox catalyst. The caustic
concentration for the circulation should be 20°Be. The catalyst concentration in the
caustic should be 100 ppm. Merox solution circulation rate should be 4 to 5 M 3/hr.

Operating pressure which is maintained by the pressure controller on the rundown


line should be about 18.0 kg/cm2 at the extractor C2. Reducing any of these
variables excepting the pressure will affect mercaptan extraction efficiency. Too low
an operating pressure favours amine and caustic entrainment in LPG stream.

 TROUBLE SHOOTING

I. MERCAPTAN EXTRACTION

Mercaptan Extraction can be adversely affected by one or a combination of the


followings :

Poor Mercaptan oxidation (This would be identified by a high Mercaptide


Concentration in the regenerated Merox Caustic. That is 'shake test" time too
long). This is the most frequent cause of poor mercaptan extraction.

A dramatic increase in Hydrocarbon Feed and/or regenerated Merox Caustic


temperature, for example, 55-60°C versus 45°C.

Increase Mercaptan content of the Hydrocarbon Feed, for example, higher


mercaptan loading or higher molecular weight mercaptan in the hydrocarbon feed.

Accumulation of non-regenerable acidic compounds or salts in the Merox Caustic.


The most obvious effect is the consumption of caustic free alkalinity. This problem
can be identified by analysing the Merox Caustic solution for % NaOH as a strong
base (U P method 209). This value should always be maintained above 10 WT.%.
Some of the undesirable compounds are H 2S ( as sodium sulfide). carbon dioxide
(as sodium carbonate), and sodium thiosulfate which is oxidised sodium sulfide.
Proper feed prewashing is essential in preventing the rapid contamination of Merox
Caustic with such compounds.Contamination are purged by replacing a portion of
the caustic inventory in the system with fresh caustic. (The concentration should
be chosen so as to keep the concentration in the Merox Caustic between 18 and
25° Be).Only plant Operating experience can determine what is the maximum
allowable concentration of each contaminant.

Upsets in extractor column hydraulics which are reflected as a marked reduction in


extractor tray efficiency, This can be caused by partial vaporization of hydrocarbon
in the extractor, improperly stalled trays, excessive hydrocarbon or caustic flows to
the extractor, etc. Partial hydrocarbon vaporization is the result of increased feed
temperature or the inclusion of lighter compounds in the charge stock and/or
lowering of extractor operating pressure. An upset in column hydraulics is
evidenced by excessive caustic carryover with the extracted hydrocarbon into the
caustic settler.

II. MEROX CAUSTIC REGENERATION


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Improper Merox Caustic Regeneration is caused by one or a combination of the
following :

Air Injection is insufficient. Insufficient air injection is quickly ascertained by noting


the oxygen content of the Vent Gas from the Disulfide Separator. A value of less
than 8 Vol. % Oxygen would confirm that insufficient air is being injected. However,
this should be confirmed by a "Shake Test" of the lean Merox Caustic or by
Laboratory Analysis of the lean caustic for Mercaptide (and Sulfide).

Immediately check the Air Injection System to verify that air is flowing to the
Regeneration Section at the rate previously established. If there is reduced or no
air flow, re-establish proper air flow. However. if air injection is found to be at the
previously prescribed rate, then lack of sufficient regeneration air is probably due
to :

III. SULFIDE CONTAMINATION

A lead acetate paper check on the prewash hydrocarbon stream will determine if
sulfide contamination is happening and determine its relative severity. If the
presence of H2S in the extractor feed is confirmed, necessary steps must
immediately be taken to re-establish proper hydrocarbon/DEA and prewash
operation.

Increase air injection in 10% increments. If there has been a sudden decrease in
the Vent Gas Oxygen concentration (for example: 8 Vol. % to 4 Vol. %). the cause
is likely to be massive sulfide contamination. It may be impossible to inject
sufficient air to oxidize all the sulfide on its initial pass through the regeneration
system. In this case air injection should be increased to its maximum value. It may
be necessary for the sake of expediency to permit the oxygen content to go higher
than normal. Maximum air is limited to maximum flow meter and control valve
capacity. The disulfide separator pressure control valve should be monitored in this
case. Maximum temperature at the oxidizer outlet should be 60°C. The inlet
temperature should be 50-60°C or as high as required without allowing the outlet
temperature to exceed 60°C. Samples of the rich and lean Merox Caustic should
be sent to the Laboratory for Mercaptide and Sulfide Analysis.

Since the oxidation of sulfide is an exothermic reaction substantial sulfide


contamination is evident if temperature rise greater than 3°C is noted across the
oxidizer. It may be necessary to note only increase in oxidizer temperature and
pressure, but also begin purging the contaminated Merox Caustic from the system
when this is done, be sure to make up with fresh caustic of the correct
concentration. Proper amount of catalyst should also be added.

Continue taking these appropriate measures until the prewashed Hydrocarbon is


free of H2S and the rich Merox Caustic contains less than 3000 WPPM Sodium
Thiosulfate Periodic Analysis of rich and lean caustic as well as check on the Vent
Gas Oxygen content will indicate when the sulfide has been completely oxidized to
thiosulfate and proper Mercaptan Oxidation is re-established. At this time re-
establish normal oxidizer temperature and air injection conditions. Slowly add extra
merox catalyst to the system over a four hour period.
- 61 -
On the other hand, should sulfide contamination be verified but the source quickly
eliminated and the rich merox caustic analysis confirm low sulfide contamination.
e. g. less than 3000 PPM Na 2S2O3 immediately add some merox catalyst. say 1
litre of WS to the system. The air injection rate may be increased at 10% intervals
(to maintain ( 8 -12 Vol. % oxygen in the Vent Gas) and Oxidizer inlet temperature
increased so that the regeneration system will recover in five to twenty hours.

IV. INCREASED SYSTEM MERCAPTAN LOAD

If various checks outlined previously indicate the absence of sulfide contamination,


insufficient regeneration air is due solely to increased hydrocarbon flow and/or
increased system mercaptan concentration resulting in increased feed mercaptan
loading. In any event, with increased air injection and temperature, the
regeneration system will recover rapidly. Additional catalyst make up may be
considered at this time. Merox Caustic flow to the extractor and increased air
injection should have been increased proportionately with any increase in
Mercaptan loading from increased hydrocarbon feed rate.

V. MEROX Catalyst CONCENTRATION IS INSUFFICIENT

Insufficient Merox Catalyst in the oxidizer and caustic solution is confirmed by the
lean Merox Caustic Mercaptan concentration greater then 200 WPPM (or the
"Shake Test" time of longer than 90 sec), when the Vent Gas Oxygen content is
greater than 19%. This may be further confirmed by noting the physical
appearance of the lean caustic. Lack of catalyst will leave the caustic solution pale
green or even relatively colorless. If this situation exists, add 1 bottle of Merox WS
over an eight hour period.

Frequently the problem is not too little catalyst or increased catalyst consumption,
but improper addition of merox catalyst. To prevent any loss of catalyst (usually at
the disulfide/caustic interface in the disulfide separator). A special effort should be
made to always add make up catalyst slowly and to mix it well to obtain a more
uniform catalyst distribution. Also never over-oxidize the Merox Caustic (evidenced
by blue rather than green lean Merox Caustic). For this decrease the disperisibility
of the Merox Catalyst causing catalyst loss.

VI. OXIDIZER TEMPERATURE IS TOO LOW

The normal recommendation for the LPG Merox Unit is to maintain the Oxidizer
Inlet temperature at the minimum required in the range of 38-45°C. Above 45°C,
over oxidation reactions can actually lead to acid generation causing further
caustic neutralization. However this temperature may be increased to 50-60 oC in
instances requiring sulfide oxidation.

VII. EMULSIFICATION AND CAUSTIC ENTRTAINMENT

Merox Catalyst Caustic Solution does not increase the tendency of caustic solution
to emulsify with Hydrocarbon. It does increase the detergent or foaming properties
of caustic. Consequently, dirt and scale in equipment will be dislodged by Merox
Caustic. Part of this dirt or scale may consist of iron sulfide. Therefore, equipment
- 62 -
which is new or long out of service should be thoroughly flushed and cleaned
before being commissioned or it may be necessary to discard the first batch of
caustic if it becomes subsequently loaded with iron sulfide scale from improperly
conditioned equipment.

Also, certain corrosion inhibitors or the acid treatment of the inhibitor, promote
emulsion problems The inhibitor is picked up by the Merox Caustic from the LPG
being treated. The presence of inhibitor or excessive concentrations of inhibitor
can normally be traced to improper inhibitor injection and thus with proper additive
control, the problem can be eliminated.

VIII. INADEQUATE DISULFIDE SEPARATION

Poor disulfide separation from the lean Merox caustic in the disulfide separator can
be caused by surfactant materials, which keep the disulfide suspended in the
caustic. Disulfides in the Merox Caustic can be analyzed by UOP Method 393.

The presence of surfactants in the lean Merox Caustic can be determined by a


surface tension test comparison between plant and fresh Merox Caustic. Plant and
Fresh Merox Caustic are each shaken with equal volume of isooctane. The time
required for the hydrocarbon-caustic phase to separate completely is noted in each
case.

Significant difference in surface tension and settling time is indicative of the


presence of surfactant in the caustic. The settling time for the plant Merox Caustic
will be significantly longer if surfacants are present.

If the Merox Caustic is not sufficiently regenerated when leaving the oxidizer, some
further mercaptan to disulfide may occur in the settling compartment of the
disulfide separator down stream of the coalescing section. Any disulfide formed
there will not have been coalesced into sufficiently large droplets to gravity
separate from the caustic and will remain suspended.

Comparison of the Mercaptan content of the Caustic sampled at the oxidizer outlet
and disulfide separator caustic outlet will indicate the Mercaptan are oxidizing to
disulfides in the disulfide separator settling compartment. This is usually caused by
insufficient merox catalyst. or mixing. Slowly add extra Merox Catalyst and take
steps to keep the Merox Catalyst suspended will eliminate this problem.

If insufficient separation is suspected, a Laboratory Coalescing Test can be


conducted to check if dislfide separation could be improved. Insufficient separation
is likely to be caused :

Improper installation of coalescing partition so that anthracite coal has migrated.

Improper installation of anthracite coal, or

No anthracite coal at all.

At the earliest opportunity the vessel should be opened and the situation verified
and corrected. Proper disulfide removal from the lean Merox Caustic is imperative
- 63 -
if full benefit is to be received from the extraction operation. All of the disulfide
cannot be gravity separated from the regenerated caustic. A low re-entry sulfur
concentration (less than 10 PPM in the Hydrocarbon) is considered adequate.

IX. INADEQUATE PREWASHING

Aside from the obvious cause associated with the break-through of acidic
compounds due to excessive quantities of H 2S or CO2 in the feed or Spent
Caustic, the only remaining cause for a problem is inadequate contacting or mixing
in the prewash. This is caused by insufficient hydrocarbon flow. Hydrocarbon
distribution into the batch caustic is insufficient to assure proper mixing and
contact. This situation can only be corrected by plugging some distributor holes.
The number of holes to be plugged should be propertionate to the decrease in
feed rate.

- 64 -
7. U-25 CRACKED FCCG MEROX

 UNIT CAPACITY

Cracked Naphtha Merox Unit is designed to Process 300,000 T/Yr.of cracked


gasolene and Straight Run gasolene; the LSR component being 60,000 T/Yr. The
Unit Shall operate for 345 on stream days in a year.

 FEED SPECIFICATIONS

(i) Boiling range TBP oc C5 -90


(ii) Sp. Gravity at 15.6°C 0.67
(iii) Total Sulphur wt. ppm. 100 max.
(iv) Mercaptan Sulphur wt. ppm 850 "
(v) H2S wt. ppm 10 "
(vi) RVP : Kg/Cm2 0.7 "

 PRODUCT SPECIFICATIONS

The Merox treated gasolene shall meet the following specifications :

(a) Copper strip corrosion (3Hrs.at 50°C) 1 Max ASTM


D-130-65
(b) Mercaptan'S' wt. ppm 5 Max
UOP -163
-62
(c) Oxidation stability minutes 390 min.
ASTM D -525
-55

 TYPE OF CATALYST USED

Caustic dispersible Merox(catalyst WS supplied by Universal Oil Products


Company, Illinois USA, is used in the sweetening Reactor 25V2 of this unit. Initial
charge of catalyst about 3kg of active ingredient of catalyst. Whenever caustic
solution is replaced, catalyst make up is necessary. Normally we use 12M 3 of
NaOH of 8% concentration. The catalyst make up is 1 kg. of active ingredient for
every 4 KL of caustic.

When the circulating caustic becomes more than 50% spent, the entire caustic
should be discarded to Effluent Treatment Plant and fresh catalyst should be taken
in as detailed above, followed by addition of fresh catalyst to the caustic.

 DETAILED DESCRIPTION OF P&ID

Merox treatment of SRN and FCC gasolene consist of

Caustic prewash
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Liquid-liquid sweetening
Caustic settling
Passing through sand filter

Caustic prewash is provided on for straight Run naphtha, as FCC Gasolene after
stripper and Debutaniser contains little or no Hydrogen Sulphide. For sweetening
proper a mixer type of Reactor has been provided. Post treatment consists of a
caustic settler and sand filter. Anti-oxidant injection facility is also provided.

Straight-run naptha stabilisation from distillation unit stabiliser is "charged to the


unit by feed pumps 025 P2 A&B. The flow-rate is controlled by 025 FRC-1. and is
taken into caustic prewash vessel 025 V1 {100 x 600). There are three inlet
nozzles and a stainless steel wire mesh at the top as in other prewash vessels.
Caustic is to be changed out as indicated by its strength.

FCC gasolene from gas concentration section stabiliser bottom joins straight run
naptha at the outlet of caustic prewash vessel and the mixture goes to the merox
Reactor. The flow of FCC gasolene into merox is recorded by 025 FR 14. The
combined flow of naphtha and gasolene is recorded by 025 FR 4. Caustic with
suspended merox Catalyst No.2 is added to combined hydrocarbon under 025
FRC 10 flow control. Air required for oxidation is added to the combined stream
plus caustic through a special check valve 025 y 1 which ensures thorough mixing
of air and hydrocarbon. Air flow rate is controlled by 025 FRC 5.

The reactor 025 V2 (1600 x 6100) is a liquid-Iiquid sweetener effected in a mixer


vessel having perforated trays to achieve intimate mixing of hydrocarbon and
caustic containing suspended merox catalyst in order to accomplish desired
sweetening reactions. Each tray has a total of 62 perforations distributed evenly at
four different radial distances. The tray joints are all fixed with neoprene gasket to
avoid any leakage at joints which would affect mixing efficiency. The mixture of
hydrocarbon, air and caustic containing catalyst rises up the mixer through the
perforated plates and exits at the top of vessel and goes to caustic settler vessel
025 V3 (2400 x 9000).

The mixture enters the settler through a vertical slotted pipe distributor. The
hydrocarbon leaves from the top of settler to sand filter 025 V4 (2200 x 4800).

The caustic containing merox catalyst settling down at the bottom of settler is
withdrawn through a perforated riser pipe having 50 Nos. 7/8" holes placed
circumferentially in a spiral fashion. The riser pipe ensures withdrawal of clear
caustic from the settler for circulating back to feed. The settler caustic is pumped
by pump 025 P1 A&B and circulated under flow control 025 FRC 10. For addition
of catalyst into circulating caustic stream, when necessary catalyst addition may be
done through the pot 025V5 (450x900) by pushing the catalyst solution by air
pressure.

The hydrocarbon enters the top of sand filter through a distributor pipe assembly
with holes drilled to a specified pattern. The sand packing is provided in the top
half portion of vessel and supported at the level. Hydrocarbon filtering out of the
sand bed is picked up from a high enough level to ensure clear hydrocarbon
withdrawal. The treated product is sent to storage after maintaining the necessary
- 66 -
back pressure in the unit by 025 PIC 12. Injection of UOP No.5 antioxidant with or
without copper deactivator is done by dozing pumps (23P-3A/B/C/D) located in unit
023. A slip-stream of run-down product acts as a carrier for inhibitor discharging
from the dozing pump. Sand filter is provided with a bypass. Excess unreacted air
accumulating on top of sand filter can be vented from the floor level itself by the
extended vent line. Facility also exists for back washing the sand-bed, if required.

The treated product from the unit is a component of motor gasolene pool.

NOTE: LSR gasolene is now not processed in 25 unit. 25V1 is being used as
knock out pot for sponge gas from 20-C-2 to 20-C-6.

25-P-2A/B have been removed to other services and gasolene inlet and outlet
lines have been blinded.

 PRE-COMMISSIONING OPERATIONS

I. CHECKING COMPLETION OF CONSTRUCTION WORK, INSPECTION


AND BOXING UP OF EQUIPMENTS.

The following preliminary operations will have to be carried out to ensure a


successful start-up of the unit :

Check that all mechanical work of construction have been completed. All
equipments and pipelines must be inspected and tested hydraulically at stipulated
pressure depending on design conditions. They are to be boxed up only after
internal inspection for proper fittings and cleanliness. Finally, all unit equipments
and lines are to be signed off as complete in all respects in the Production Deptt.
check lists made for the purpose.

Make a final blind list indicating which should be in position and taken out before
starting gas purging operations. Ensure that all blinds have been installed at the
proper sides of valves and signed off in the list.

Check and ensure the availability of Fire-fighting and safety equipment in the unit
area in good working condition.

Ensure all utility systems and flare release header is in service and ready for use.

Check that free movements inside the unit area are not obstructed by scaffoldings,
construction debris, tools etc. Get them cleared away from the unit area.

Isolate the unit from other plants and storage tanks at the unit limits with block
valves, for carrying out flushing and purging operation.

Isolate to remove instrument orifice blocks for flushing purposes.

II. WATER FLUSHING OF THE UNIT

Water flushing of the entire unit has to be done with all pumps running on line so
that all muck, scale and construction debris are washed out of all equipments and
- 67 -
lines. For this purpose, the unit can be conveniently divided into sections and
individual equipment wise water flushing can be done, Temporary fire water hose
connections are made on unit equipment or lines at suitable points and thorough
flushing is done. Suitably wire mesh strainers are to be installed on pump suction
spools during the water flushing operation to protect the pumps from damages.
The pumps are to be run at least for 24 hours continuously to ensure their free and
smooth functioning. During the water flushing operations, care should be taken to
see that pump discharge valves are sufficiently throttled so as not to overload their
motors. The suction screens installed will have to be opened up and cleared of all
debris collected periodically after stopping the pumps, This type of cleaning the
screens will have to be continued till they remain free of any muck continuously at
least for 8 hours.

On completion of water flushing the unit equipments and lines satisfactorily, we


have to pressure test entire system with steam.

III. PRESSURE TEST & PURGE EQUIPMENT AND LINES

In order to check for leaks on equipment and lines after water flushing they are all
tested with steam pressure of about 5 kg/cm2 proceed as follows :

Block off caustic circulation pumps Pl A & B with their suction, discharge valves.

Open wide all vents and drains in vessels Vl, V2, V3. Isolate sand filter V4 closing
off its inlet and outlet valves. The sand fi1ter is to be purged with gas and tested
under gas pressure to avoid caking of the sand bed.

Hook up steam hoses to the steam out connections of the vessels Vl, V2 and V3
and back up steam into the vessels and lines upto the unit limit block valve.

After sufficient steam purging for about 15 minutes from all possible vents and
drains. Close these points and pressure up the system to about 5 kg/cm2 with
steam. Check up the entire unit for leaks and get them attended.

After successful completion of pressure test. continue with steam purging of the
unit system till all air from equipment and lines have been removed. The system is
ready for taking in hydrocarbon when all air from the system has been displaced
by steam. Maintain a positive pressure of steam till fuel gas is taken into the unit
and it is pressured up with gas.

Fuel gas is slowly taken into the pre-wash vessel V1 and then to mixer V2 and
caustic settler V3. The sand filter is also purged with gas first to displace all air and
then pressured up to fuel gas system pressure. Catalyst addition pot V5 must be
isolated from the gas purging lines. Drain all steam condensate from low points
and drains. When gas smell comes out of the vents of the vessels. steam can be
completely shut off and system allowed to remain at 0.5 kg/cm2 pressure of fuel
gas.

- 68 -
IV. CHARGING OF CHEMICALS AND CATALYST

Before actual start-up of the unit, the treatment systems should be made ready to
receive LSR gasoline from AVU. Prepare system as below:

Pump in 10°Be caustic solution from storage tank in Kero Merox section and
establish working level in the prewash vessel V1.

Charge 10oBe caustic solution into caustic settler V3 from Kero Merox section till
sufficient level is obtained in the settler for circulating caustic through mixer V2.

Prepare Merox catalyst slurry in catalyst addition pot V5. taking desired quantity of
catalyst in it with caustic and water to make the solution. Keeping the vent of V5
open. Add air through the air connection to the pot for proper mixing of the slurry.
Then close the vent and increase the pressure in the pot, to blow the catalyst
slurry into the system along with the caustic solution circulated through the mixer
V2. Care should be taken not to blow air into the system to avoid explosion. The
catalyst is blown into the system alongwith caustic circulating after introducing
gasoline feed in the unit. Catalyst addition to the system has to be done in batches
depending on the doctor test conducted on the treated gasoline.

Make ready the anti-oxidant injection facility in visbreaker Naphtha Merox section
for dosage into the treated gasoline stream from the unit, before it is routed out to
storage tanks.

 START-UP PROCEDURE

When pre-commissioning operations in the unit have been successfully completed


and the entire system is under Fuel gas pressure then Hydrocarbon can be taken
directly into the unit. Confirm straight run gasoline from AVU is ready to be
supplied for Merox treatment proceed further as follows:

Fill up with straight run gasoline the unit vessel, viz., prewash vessel V1, mixer V2,
caustic settler V3 and Sand filter V4, one by one which have been kept under fuel
gas presssure. Pressure up each vessel to about respective operating pressure.

Prepare Merox catalyst slurry in catalyst addition pot V4 and keep it ready for
blowing into the circulating caustic solution to the mixer V2.

Inform Kerosene Merox section and charge 10 oBe caustic solution from there to
the prewash vessel V1 and bring up normal operating caustic level.

Transfer caustic solution with the help of circulation pumps P1 A/B to the mixer V2.
Commission flow controller to regulate the flow to mixer.

Commission injection air system from kero Merox unit and start air injection to the
mixer at specified rate on FRC control.

- 69 -
Commission gasoline charge pumps and commence flow with FRC-on line through
the mixer V2 after prewashing stage in V1 Route gasoline to storage passing
through settler V3 and sand filter V4, with the pressure in service.

Start injecting the required quality of merox catalyst into the caustic stream going
to the mixer V2, taking care not to blow air into the system.

Bring operating conditions to normal. When cracked gasoline becomes available


from GCU, charge it to the mixer V2.

Start anti-oxidant injection into the treated gasoline stream at the stipulated rate.

The above procedure was applicable when 25V1 was used as prewash vessel.
Now 25V1 is being used as the additional Knock Out Pot for the sponge gases
from 20C2 to 20C6. LSR naphtha from AVU is not processed in 25 Unit.

When the precommisioning operations in the unit have been completed and the
unit is under fuel gas pressure, confirm CR gasoline from FCC is ready to be
supplied for merox treatment proceed as follows :

prepare merox catalyst slurry in the catalyst addition pot 25V5 and keep it ready
for blowing into the circulating caustic solution to the mixer 25V2.

Charge 10oBe caustic solution into 25V3.

When cracked gasoline becomes available from GCU charge to the mixer V2.

Transfer caustic solution with the help of 25P1A/B to the mixer 25V2 . commision
controller 25FRC10 to regulate flow.

Commision air injection system and start air injection to the mixer at specified rate
on 25FRC5 control.

Start anti-oxidant injection into the treated gasolene stream.

 SHUT DOWN PROCEDURE

Before commencement of the shutdown, stop antioxidant injection to the gasoline


stream. Then inform all concerned of intention to shutdown the plant and proceed
as follows :

Shut off air injection to mixer V2 and block off the valves.

Stop cracked gasoline to mixer V2.

Close of pressure controller (25PIC-12) on the gasoline rundown line an hold


system pressure. .

Pump out caustic from settler V3 and mixer V2 to the disulphide separator or to
spent caustic disposal system.
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Displace all gasoline from the vessels to the storage or slop tank with fire water.
Finally drain all the water and hydrocarbons from the vessel taking care not to pull
any vacuum in them.

Isolate vessels with blinds and steam them out thoroughly using the steam out
connections provided. Drain all condensate from low points.

Maintain upto date record of blind list.

Water wash the caustic vessels and sand filter and mixer with fire water repeatedly
till they are free of chemicals and clear water flow out from the drains freely.

Make sure that individual equipment has been properly isolated by blinds and
made gas and chemicals free, as per laid down procedure. Conduct a gas test
before allowing entry inside a vessel. Insist on protective equipment being worn by
personnel entering in vessels in caustic and other chemicals service.

 EMERGENCIES

I. POWER FAILURE

If it is a general power failure, all the pumps in the unit will stop. Feed to the unit
will also be interrupted. In this case the plant has to be shutdown. Follow the steps
given below:

Shut off air injection to mixer V2.

Close off the discharge valves of all pumps which have stopped.

Shut off pressure controller at unit limits and hold pressure in the system, till power
supply is resumed.

Start-up the unit, as per standard procedure as soon as power supply is restored.

II. STEAM FAILURE

If feed supply to the unit is interrupted due to general steam failure; unit will have
to shutdown and wait for resumption of feed supply from AVU/GCU. If it is a local
failure gasoline Merox treating section can continue to run, as long as possible.

III. COOLING WATER FAILURE

The unit will have to be shutdown as pumps cooling water supply will be affected.
as well as feed supply from AVU/GCU.

IV. INSTRUMENT AIR FAILURE

Air failure will result in all the unit control valves operating in their fail safe
positions. i. e., they will all close. If feed supply is interrupted unit will have to
shutdown. Otherwise unit can be operated with the control valves blocked off and
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maintaining pressure and flows on bypass. Levels in vessels will have to be
monitored till air supply is restored.

V. UTILITY AIR FAILURE

If the failure is only for a short duration unit operation can be continued normarly.
In the absence of oxidising air injection, the mercaptan conversion efficiency drops
off quite rapidly. Hence, the product will have to be slopped as soon as it is doctor
positive. Normal operations can be reverted to when air injection is restarted and
the product is on grade.

 OPERATING VARIABLES

In the mixer V2, all heavier mercaptans are converted to disulphides. Here, the
operating variables are air injection rate, Merox catalyst concentration in caustic
solution and circulating caustic strength. Air injection rate should be @ 1.75
NM3/kg of sulphur converted. Too much air will give rise to continuous venting from
the sand filter V3 and increases the fire hazard. Merox catalyst concentration
should be 100 ppm in the caustic solution Caustic circulated should be 10-20 deg.
Be.

Operating pressure of the Mixer is about 8.4 Kg/cm2, Hence, the pressure
controller will have to be set accordingly to give the desired back pressure in the
mixer.

 MODIFICATIONS

1. SR Naphtha from AVU is not treated in 25 unit as 25 unit capacity is being


utilised with CR gasoline. To remove light mercaptans which can be removed in
prewash, modification was done to route part of CR gasoline to 25V1.

2. Facility to use 25V1 as additional knockout pot for sponge gas from 20C2 to
20C6 gasoline inlet and outlet kept blinded.

3.
Name of the Scheme Scheme for butane blend in MS

Scheme No MR/PS/300/2002/4

Scheme implemented Apr’03


on
Description of Provision of routing of butane rich streams from
Scheme Depropaniser bottom in PRU to FCCG line at the
downstream of backpressure control valve in Merox.
Reason for Butane stream addition is a very good media to
modification increase octane. This can be added to MS subject to
meeting the RVP/VLI limit. Thus octane boost
obtained after butane addition would be used to
upgrade naphtha to MS.
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Operating instructions 1. Butane rich stream from 18C1 bottom is blended into
U-25 R/D to boost the Octane of MS. This also helps in
upgradation of additional Naphtha into MS. The
blending is done through a new control valve 25-FIC-
1109, provided at the downstream of U-25 BPC.

2. Butane blend into MS also poses some hazards like


addition of more butane into MS can lead to MS quality
failure in RVP & VLI and can also lead to potentially
dangerous situation in MS tank.

3. Interlocks provided in butane blend facility are :

 25-FIC-1109 would close at 18C1 bottom temp less


than 92 Deg C.

 25-FIC-1109 would close when 25-FR-4 ( FCCG


flow to Merox ) falls below 10 m3/hr.

4. 25-FIC-1109 would normally remain on ratio control.


Ratio would be set between 0.04 -0.07. This means
butane flow would be 0.04-0.07 times sum of
Reformate and FCCG flow. But this facility is yet to be
created.

5. At present , 25-FIC-1109 would remain on Auto and set


point has been locked at 6 M3/hr (max). This means at
all times when the control valve is on auto, the butane
blending can be set at a flow equal to or less than 6
M3/hr.

6. Please stop butane blend in the event of


following :

 No Reformate rundown from CRU


 No FCCU gasoline rundown (Interlock has been
provided on this and blending control valve should
automatically shutdown)
 Upset conditions in PRU

7. Butane in Total MS pool (Reformate+FCCU


gasoline+OHCU Naphtha+VBN) should be limited to
3.5-4.0%w

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8. SAFETY & FIRE FIGHTING FACILITIES

All the general safety rules and practices applicable to Petroleum Refinery
operations are to be followed in Merox Treating Plants also. Additionally some of
the safety precautions to be taken in each case are presented below:

I. CHEMICAL HANDLING

Chemicals, Amine & Caustic are used in this unit. Rubber gloves, aprons and face
shields are supplied for any job in the chemical area of this unit and they should be
used for any job here. Any spillage of chemicals on the body can be washed off
with copious amounts of water. A safety shower is provided in Merox Units for any
chemical spillage-emergency on the body of any person. All safety equipment
should be cleaned with water so that they can be safely re-used later on.

CAUSTIC SODA:

Caustic solution, commonly called lye, used in Merox units is to be handled


carefully with due precautions. Gloves, Goggles and face shields must always be
used in the treating area for any job. Painful injury and possible blindness can
result out of caustic splash into the eyes. A safty shower is provided in the treating
area for washing the body immediately if an accident occur. In case of caustic
splash into the eyes, both the eyes must be thoroughly washed with plenty of
water and the person should be sent for firstaid. All eye injuries must be referred to
proper medical attention after the first aid.

Workmen should be made aware of the fact that caustic does not give immediate
warning of its presence on the skin by burning or irrit3tion. But its presence on the
skin can be recognised by its slippery, soapy feeling. A doctor must be consulted
immediately in case of a severe skin burn. In view of the hazards mentioned
above, workmen must wear rubber gloves and apron besides goggles and face
shields when working in an area exposed to caustic. Caustic is destructive to
leather and it is advisable to wear rubber footwear also while handling caustic.

when caustic comes into contact with the skin, the area must immediately be
washed with plenty of water. Depending upon the severity of exposure, washing
with a 2% solution of acetic acid can be followed. Fecilities for immediate washing
with water like safety shower must be readily available in the caustic handling
area. Pumps, valves and process equipment scheduled for maintenance must be
flushed thoroughly with water prior to opening. Maintenance workmen must wear
all protective equipment while doing jobs on equipment in caustic service.

CATALYST :

Merox catalyst has no harmful effect on the skin. However, workman should be
advised not to contaminate any part of their bodies with catalyst. Should any
contact takes place, the catalyst must be carefully washed off the skin with copious

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amount of soap and water until the blue colour is no longer seen. Catalyst should
not be taken internally nor breathing of its dust permitted.

DISULPHIDE

Disulphides are high boiling oily organic liquids having sp. gravity from 0.95 to
1.06. They have an obnoxious odour of onions. They may cause skin irritation and
hence contact with skin should be avoided. No data is available about their
dangerous properties. They should not be consumed. They are insoluble in water,
but can be washed of the skin with warm water and a good detergent. Clothes
contaminated with disulphides must be removed from the body. Breathing of their
vapors is also not allowed.

AMMONIA

Ammonia gas leaks will be pungent and are easily detected by smell. The cylinder
should be immediately shut off. Ammonia gas is highly soluble in water and at low
concentration of 0.2 wt %, it does not present any critical safety problems. If there
is a spillage of Ammonia solution on the body, it should be washed, off with plenty
of fresh water.

For storage and handling methanol all the safety precautions as applicable to
gasoline should be followed.

II. FIRE FIGHTING FACILIITIES :

Portable Dry powder extinguishers and Foam extinguishers are kept at various
locations in the Units and can be used for all small fires.All the Merox Units are
provided with two parallel fire water mains one on east and another on west side.
The normal pressure in these mains remains at 2kg/cm 2 and in case of fire, this
pressure can be boosted upto 10 kg/cm 2. Fire water monitors which are provided
on the mains can divert the water jet to any angle we require and can be used for
fire fightingDry powder extinguishers, and foam extinguishers of portable type are
provided in the unit at different locations for fighting small fires.For fighting bigger
fires, fire water is available in the unit which is surrounded by fire water mains. The
normal pressure in the mains is about 3 to 4 kg/cm2.

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