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INDEX
S. NO. DESCRIPTION PAGE NO.
1.0
1.1
1.2
2.0
2.1
2.2
2.3
2.4
2.5
2.6
2.7
2.8
2.9
2.10
3.0
4.0
5.0
6.0
7.0
General
Introduction
Glosssary
Plant Description
Design asis
Process Description
!"uip#ent Description
Process Principles
$i#pli%ied &lo' Diagra#
(aterial alance
)nit *ayout Plan
&eed and Product $peci%ication
)tility Description
)tility condition and re"uire#ent
Interconnecti+ity
Preco##issioning ,cti+ities
-or#al $tart)p
Process /ariale
-or#al $utdo'n.
!#ergency $utdo'n Procedure
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8.0
9.0
10.0
11.0
12.0
12.1
12.2
13.0
14.0
15.0
16.0
)nit Protection $yste#
*aoratory e"uire#ents and $cedule
!"uip#ents and Instru#ents $u##ary
$pecial Procedure
eactor ot ed asing.
atalyst ei#pregnation
*ist o% $pecial !"uip#ents.
roule $ooting
e#ical onsu#ption During Initial and -or#alperation.
&ire $a%ety
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CHAPTER1
GENERAL
1.1 INTRODUCTION
Petroleum distillates normally contain small amount of mercaptans
(organic sulfur compounds) which impart obnoxious odour to the
product.
The LPG feed from FCC and elayed Co!er may contain some
mercaptans" but most of them are formed during crac!ing reactions.
#ercaptans are also formed when sulfur compounds decompose or $ %&
and ole'ns react. #ercaptans may be al!yl or aryl in nature.
P #erox process is an e*cient and economical catalytic process for
the treatment of light hydrocarbon products . This process is used forthe con+ersion of mercaptan sulfur to another less ob,ectionable form
of sulfur compound or remo+e the mercaptan sulfur from the
distillates. The P #inal! nit (#inimum -l!ali) is employing a
sweetening process to oxidie mercaptans to disul'des using air as the
source of oxygen. This reaction proceeds at nominal temperature in
presence of a catalyst in al!aline en+ironment.
#erox treatment has the following ob,ecti+es
1. To impro+e lead susceptibility of light gasolines
1. To impro+e the susceptibility of gasoline to oxidation inhibitors
1. To impro+e the odour of the products
2. To meet product speci'cation
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1.2 GLOSSARY
aeotrope a mixture of substances that beha+es as a single
substance in that the +apor produced by partial
e+aporation has the same composition as the
li/uid.antioxidant chemical additi+e to inhibit oxidation reaction.barrel 0% .&. gallons measured at 123F4P barrels per day (also 4P&)caustic sodium hydroxide solutionC5$ caustic5hydrocarbon +olume ratiodisul'de class of sulfur compounds characteried by a
sulfur6to6sulfur bond and relati+ely low +olatilityrepresented by the general formula 7&&7.
8P endpoint (-&T# distillation).extraction remo+al of mercaptan sulfur from hydrocarbon.GC or GLC gas chromatographygph .&. gallons per hourgpm .&. gallons per minutegum polymeried hydrocarbonhydroperoxide compound responsible for propagation of gum
forming chain reaction (6$)
94P initial boiling point (-&T# distillation)inhibitor compounds responsible for delaying or
terminating a chemical reactionL$&: li/uid hourly space +elocitymercaptan common name gi+en to class of compounds
ha+ing thiol functional groups represented by the
general formula 7&$naphthenic acid organic (carboxylic) acid;m< normal cubic meter ( = atm. 23C)std. m< standard cubic meter ( 9 atm. =>3C)organo6metallic complex compound characteried by wea!
carbon to metal bondsP? prewash
re6entry sulfur entrained disul'de sulfur in regenerated caustic
that enters and dissol+es into the exiting
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hydrocarbon product from an extractor7@ reactor&CF$ standard cubic feet per hour ( = atm. 123F)sweetening con+ersion of mercaptan to disul'de without
desulfuriation
stability /uality of a fuel to remain unchanged for long
periods of time in storagethiol sulfur6to6hydrogen bondthiophenol common name gi+en to aryl mercaptansA also the
compound C1$>&$
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CHAPTER2
PLANT DESCRIPTION
2.1 DESIGN BASIS
This unit is designed to process 6=2> deg C)
2. epentaniser bottom stream (C16=2> deg C)
3. eisohexaniser o+erhead stream (iC1)
7FG C#P;8;T&A ($ea+y #ogas) A
1. ;aphtha &plitter sidecut stream (=2> =D2 deg C)
2. $ea+y crac!ed ;aphtha stream (=D26%=> deg C)
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2.9 UTILITIES DESCRIPTION
LP STEAM SYSTEM
7efer P E 9 AG 0% 7F 0=1 =2=
- 1 header pro+ided with battery limit isolation +al+e" blind" local PG
=22" TG 2>2" C& ow indication ( F9212 )" totaliser indication ( FH9
212). #ain header di+ided into se+eral branch headers" which supply
LPsteam to the following e/uipment.
• - 1 header supplies LP steam to esuper heater
The unit is also pro+ided with =2 ;os. of LP steam utilities stations.
COOLING WATER SYSTEM
7efer P E 9 AG 0% 7F 0=1 =%=
- =% cooling water supply header pro+ided with battery limit isolation
+al+e" blind" local PG =2
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• - D I Cooling water supply header is pro+ided to Gasoline Cooler
;o.= (&>=)" &>%" &>0). &ame sie of return header is pro+ided.
POTABLE WATER DISTRIBUTION SYSTEM
7efer P E 9 AG 0% 7F 0=1 =%%
-
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- 1 cold condensate header pro+ided with battery limit isolation
+al+e" local PG =2" TG 2>>" C& ow indication ( F9 21< )" Flow
recorder ( F7 21< ).
The main header ser+es cold condensate to the following points.
• - 0 line to water heater ( J >% )
• - 0 I line to Caustic storage tan! ( #T 7F0=16 2= )
UTILITY WATER SUPPLY SYSTEM
7efer P E 9 AG 0% 7F 0=1 =%%
- % potable water header pro+ided with battery limit isolation +al+e"
local PG =21.
The main header ser+es tility water to the following points.
• To pump seal P 2= -. ( M I line).
•
To pump seal P 2= 4. ( M I line).
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The unit is also pro+ided with =2 ;os. of utility water stations.
(UEL GAS SYSTEM
7efer P E 9 AG 0% 7F 0=1 =
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- = K I header is supplying air to Caustic storage tan!(#T67F0=1 62=)
The unit is pro+ided with =2 ;os. of plant air utility stations.
NITROGEN SYSTEM
7efer P E 9 AG 0% 7F 0=1 =0=
- % plant air header pro+ided with battery limit isolation +al+e" local
PG =2D.
#ain header di+ided into se+eral branch headers" which supply
;itrogen to the following e/uipment.
• - = header supplies ;itrogen to 7eactirs (72="7%=) and for 7
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The unit is pro+ided with = ;os. of breathing air utility stations.
INSTRUMENT AIR SUPPLY SYSTEM
7efer P E 9 AG 0% 7F 0=1 =0%
- % instrument air header pro+ided with battery limit isolation +al+e"
local PG ==2.
:arious instrument air tapping are ta!en from this header.
LP (LARE AND RELIE( SYSTEM
7efer P E 9 AG 0% 7F 0=1 ===
- =D are header pro+ided in the unit enters LP are !noc!out drum
( 0=> : = ). The header is pro+ided with battery limit blind" isolation
+al+e(:al+e up side down)" local PG =2=.
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The P&:s E +ent etc. ..discharge to LP are header.
• P&:s on 7eactor (7 2=) =2= -54.
• P&:s on 7eactor (7 %=) =%= -54.
• P&:s on 7eactor (7 %)
P&:s on Gasoline feed cooler ;o.%
nderground main header of 1 sie pro+ided in the unit with se+eral
branch header connected to it for collecting drain from +arious points.
-ll lines are connected to headers or branch header are pro+ided with
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an isolation +al+e and spectacle blind. Following drains are connected
to main header.
• rains from &>=
• rains from &>%
• rains from &><
• rain from $:2=>" $:2=" P&: =>< and Flow ri'ce F 2>2. :2B is pro+ided
with pump P 21- E local PG 2>< which is discharging to Crac!ed slops.
P 21- motor is on auto start from C& #$& 2%2" run hours #L 2%2"
based on L9 2
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-ll lines are connected to headers or branch header are pro+ided with
an isolation +al+e and spectacle blind. Following drains are connected
to main header.
• From : 20 (% line).
• From #P 7F 0=1 P>=- (
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2., PROCESS PRINCIPLES
The word O#erox has been deri+ed from the pre'xes of
% words #87 6 Captan and @idation. The #erox process is achemical treatment of $ydrocarbons to remo+e mercaptans or to con+ert mercaptans into disul'des. The principle isbased on the ability of catalyst to promote the oxidation of mercaptans to disul'des at ambient temperature using air asthe source of oxygen.
#ercaptans are represented by general formula 7&$" where O 7 stands for hydrocarbon al!yl group and O&$ for mercaptan group consisting of sulphur and hydrogen atoms. #ercaptan concentration is represented in terms of
the sulphur in the mercaptan molecule.
#ercaptans are undesirable in 'nished petroleumproducts" due to odour" stability and total sulfur content. 9nGasoline #erox treatment a 'xed bed sweetening is used.
The #erox D catalyst (9t is an acti+ated carbon whichha+e been impregnated with #erox F 4 reagent ) which iswater insoluble is deposited on a support bed of a selectedgranular acti+ated charcoal. #erox D is loaded directly intothe 'xed bed reactor and re/uires no additional impregnation
or acti+ation prior to use. The acti+ated charcoal bedadsorbs
Phenols ";aphthenic -cids and4asic ;itrogen compounds" which aQect the con+ersion reaction. The $ydrocarbon (Gasolinee)" air" and causticare simultaneously contacted o+er a solid support(charcoal bed) in the reactors" impregnated with #eroxcatalyst. The sweetening reaction proceeds at normal re'n6ery product rundown temperature" in the presence of al!ali
and #erox Catalyst according to the following formulae.
,RSH - O2 / 2SSR - 2H2O )1+
RSH - NaOH / NaSR - H2O )2+
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M!"o0
2NaSR - 12 O2 - H2O / - 2NaOH - RSSR
)+
3aal4$
#ercaptans" react with sodium hydroxide to form sodiummercaptide and water" which is re+ersible. The sodiummercaptide is then oxidied o+er #erox catalyst" to formdisul'de" thus regenerating sodium hydroxide. The totalreaction is as followsR
, RSH - O2 / 2 RSSR - 2 H2O ),+
The disulphide is insoluble in caustic and remains inthe Gasoline.
CHAPTER 5
PROCESS 6ARIABLES
5.1 (EED STOC* PROPERTIES'
H4#"og!n $&l7#! AThe presence of sul'de suppressesthe oxidation of mercaptan" as sul'des get oxidised ata slower rate than mercaptan. $ydrogen &ul'de if present in the feed stoc! results in formation of &odium
&ul'de which gets oxidised to &odium Thiosulphate. This is a neutral salt which causes no hindrance exceptthat it consumes more caustic.Boiling "ang! A -s the end point of feed stoc! is increased the presence of catalyst poison in the feedincreases and it becomes more and more di*cult tocon+ert the mercaptan present in the feed.
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M!"3a8an A -s the concentration of mercaptan(7&$ B2 ?tPP# max) increases the ease of treatingdecreases. -lso the molecular structure of mercaptandetermines its ease of sweetening. Generally branchedsecondary or tertiary al!yl mercaptans" do not get
sweetened as easily" as primary mercaptan.
&weetening is de'ned as con+ersion of #ercaptan to dilsul'de or some other form of innocuous sulfurcompound" without actually remo+ing it.
5.2 REACTION TEMPERATURE '
The higher the temperature the easier the oxidation of mercaptan processes. 4ut in normal operation the reaction temperature of Gasoline will be !ept at 23C.
5. REACTOR PRESSURE '
&u*cient pressure ( >. !g5cm%) should be held on reac6tor to !eep air in dissol+ed form. The pressure should
be su*cient to consume all the air used whilesweetening. Channeling will ta!e place through thereactor if a separate air phase is present. Pressure dropacross reactor should be less than 2. Ng5cm%
5., AIR INECTION RATE '
-ir in,ection is controlled to pro+ide =%2 to %22 : of the stoichiometric oxygen re/uirement. The stoichiometricoxygen re/uirement is 2.DB ;#
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appropriate actions must be ta!en to a+oid thesituation. $ence air to be in,ected slowly to re/uiredle+el.
5.; AL*ALI INECTION RATE '
9n,ection of dilute caustic (
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2.2 PROCESS DESCRIPTION
Gasoline (Light #ogas and $ea+y #ogas) from #aincolumn section and nsaturate Gas concentration
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sections of the FCC ( 0=< E 0=0 ). Light #ogas isrecei+ed at Gasoline #erox 45L by a =2S line" pro+ided with bloc! +al+e and bleeder +al+e at B.2 Ng5cm%gpressure and ==%3C temperature and $ea+y #ogas at1.> Ng5cm%g pressure and B=oC.
Gasoline(Light #ogas at B= deg C and 1.> Ng5cm%g and$ea+y #ogas at ==% deg C and B !g5cm%g are coole din the
Gasoline Feed coolers (&>% and &>-54. To this
Gasoline stream < o 4e caustic from < o 4e caustic storage
tan! ((#T 7F 0=1 2=) pumped by caustic in,ection pumps
P2= - and P%= and #erox Plus (acti+ity promotor) pumped
by #erox Plus in,ection pumps P2% - and P%% are ,oined.
The caustic in,ected Gasoline is mixed with the air in a
special mixer and this air plus Gasoline mixture is sent to
7eactor 72= and 7%= where the catalytic oxidation ta!es
place. The air is supplied from air compressors in Nerosene
#erox unit. The normal ow is >
and >> deg C. The air ow is controlled by F: 2=1 for
7eactor ;o. = and F: 2=D for 7eactor ;o.%. -ir line is
pro+ided with 8& +al+es @: 22= and @:22% . ?hen the
Gasoline ow is low as sensed by FT 2=>-5 FT 2=>4 the
8& +al+e @: 22= on the air line to 7eactor ;o. = will
automatically get closed. &imilarly for the 7eactor ;o.%
F-LL 2= will trip @: 22%. To the treated Gasoline P ;o.
> inhibitor is added to increase the oxidation stability. The
pressure in the reactor is controlled by the bac!pressure
controllerP9C 22= for reactor ;o.= and by P9C 22% forreactor ;o.%
MERO= REACTOR ) R >1 +
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#erox reactors" is a +ertical +essel pac!ed with P#erox D (9t is an acti+ated carbon which ha+e beenimpregnated with #erox F 4 reagent ) catalyst. Thefunction of the acti+ated carbon is to pro+ide a +astsurface where #ercaptan" catalyst" caustic and oxygen
may come into contact for completion of the sweeteningreaction. To pro+ide the al!aline medium the charcoalis !ept saturated with caustic solution with intermittantow of caustic (
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P"o#&3 @&ali4#ercaptan A > ppm
2. E@UIPMENT DESCRIPTION '
MERO= REACTOR )R >1 +
#erox reactors" is a +ertical +essel pac!ed with P
#erox D catalyst (9t is an acti+ated carbon which ha+ebeen impregnated with #erox F4 reagent" which is notsoluble in water ). #erox reactor consists of an upperinlet distributor" lower side outlet collector and bottomdrain screen. The function of inlet distributor isdesigned to pro+ide a uniform lateral ow distributiono+er the reactor cross section. The distributor holes areoriented upward. The outlet collector and +essel drainpipes are specially constructed stainless steel andpro+ided with P ohnson screen. 7eactor bottomhead is 'lled with concrete and epoxy resin coated.
The ow of the hydrocarbon" caustic and air ischarged downward through the bed. The sweetening reaction ta!es place during" the course of mo+ementthrough the charcoal bed.
Particulates in the feed will be absorbed on and 'lteredout by the charcoal bed. $ence a hot water washing
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procedure for remo+ing foreign materials absorbed bythe charcoal is done whene+er re/uired.
9t is pro+ided with following connections A+ent 6 = ;o.1 9nlet for Gasoline feed 6 = ;o.=%outlet for Gasoline 6 = ;o.% -ir +ent 6 = ;o.0 rain. 6 = ;o. There are two safety +al+es located on the top of
the reactor P&: =2= - 5 4" which are set at =.> !g5cm% gpressure to safeguard the +essel from emergency.
ischarge of these P&:U& are routed to LP Flare.
The purpose of reactor is to allow the catalytic oxidation of mercaptans to disul'des. The +essels dimensions are >22 mm. #erox ;o.D is charcoal impregnatedwith #erox F4 reagent. The +essel has got collector of =%sie. The +essel is designed for an internal pressure of =D.!g5cm%g at 2 deg C. The :esselUs material of construction is
carbon steel. The outlet os the reactor pipe is pro+ided witha drain screen.
rain Pot ;o.= (:2%" :%%) A
The +essel dimenstions are 0>2 mm 9. and a total tangential
length of B22 mm. The +esselUs material of construction iscarbon steel. The +essel is designed for an internal pressureof =D. !g5cm%g at 2 deg C.
9nhibitor 9n,ection Tan! (:>=) A
The purpose is to store the P ;o. > inhibitor. The +esseldimensions are 122 mm 9. and a total tangential length of
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>2 mm 9. . The +esselUs material of construction is carbonsteel. The +essel is designed for an internal pressure of !g5cm%g at 2 deg C.
CHAPTER ,
PRECOMMISSIONING
ACTI6ITIES
B!o"! iniial $a" &8
8ach +essel is to be inspected for proper 'tting of internals" +al+es" pressure gauges" dial thermometer
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-ll lines are to be chec!ed to see that they conform tothe detailed piping drawing -ttention should be gi+en to location of +ents" drains" and Gauge Glasses. 8ach +esselis to be ushed with water thoroughly to ensure completeremo+al of construction debris" muc!" rust etc."
For initial commissioning ade/uate safety e/uipment"'re extinguishers" 're hose connections" emergency eye wash and showers are re/uired to be pro+ided at +ariouslocations in the plant.
Personnel protecti+e clothing li!e rubber glo+es"helmets" apron" gum boots" hand glo+es" eye goggles" earmuQs are to be supplied to the operating personnel
7eactor Charcoal Loading" initial #erox catalystimpregnation and reactor bed al!alination are to be doneprior to the start up.
,.1 REACTOR CHARCOAL LOADING
4efore to loading the charcoal into the unit" all reactorinternals should be installed and inspected. The reactor ( 72=) is a +ertical +essel designed to contain the charcoal bed upon which #erox catalyst is impregnated . The inletdistributor spray pattern should be chec!ed to ensure anade/uate distribution with cold condensate.
,.1.1 LOADING PROCEDURE
The #erox 7eactor" must be isolated from the system depressurised and blinded. The top sidemanways opened. The holes in the inlet distributor
should be protected from plugging during charcoalloading by wrapping the distributor with can+as or plasticco+ering.
- catalyst hopper with telescopic or segmented load6ing soc!" that extends approx. to the le+el of the outletcollector pipe" is mounted on the top manway for #eroxD catalyst loading. The sac! position and length are
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ad,usted as the #erox D catalyst loading progresses topre+ent any coning eQect which could later cause maldistribution of $ydrocarbon ow through bed bychanneling.
-fter the loading of #erox D catalyst has commencedand the bed le+el is ,ust slightly o+er the top of theP ohnson screen collector pipe and assembly"#erox D catalyst loading should be stopped. nce the dust has settled" someone wearing a fresh air pac! orself contained breathing apparatus should enter thereactor +ia the bottom side manway to +erify that thecollector pipe assembly has been completely submergedwith #erox D catalyst and to ma!e certain that there are no un'lled spaces present underneath any of thelaterals. The reactor bottom side manway ange
faces should be chec!ed and a new gas!et should beinstalled. -fter the manway is closed #erox D catalystloading can then be resumed" shortening the soc! asloading progresses.
?hen the top of the #erox D catalyst bed has risen uniformly to within >2mm of the inlet distributor the loading is stopped. Towards the end of the #erox Dcatalyst loading" the bed depth can be satisfactorilygauged by dropping a probe through the reactormanway. -fter the dust has settled and the bed is
+isible. Personnel entering the reactor should wearscot air pac!. 9f necessary additional charcoal may beloaded to pro+ide a le+el surface of 0>2 ## below theinlet inlet distributor centre line .
- load in diagram is attached showing the appropriateoutages and a record should be !ept of the weight" +olume of #erox D catalyst loaded.
?hen #erox D catalyst loading is completed the hopper and loading sac! is remo+ed. -lso the #erox D
catalyst bed is chec!ed for cleanliness and extraneousmatter. The distributor pipe is unco+ered and the topmanway positioned and secured on four sides.
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,.1.2 DISPERSION O( MERO= CATALYST IN AMMONIA WATER
The following formula used is to calculate the /uantity of ammonia re/uired for carrying out the reim6
pregnation. - V 2.22% ? (T 6 2.% L W 51) (2X additional -mmonia.
nhydrous -mmonia is used for impregnation5reimpregnation before handling ;$
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&ha!e the #erox F4 container to disperse any re6agent that may ha+e settled and pour the contents directly into the drum upto => Ng" 1 bottles of %.> Ngeach of #erox reagent may be added to the drum at onetime. 9f more than => Ng of reagent is re/uired the
reagent should be added in e/ual batches of => Ng each. The recommended /uantity of #erox F4 reagent" is approx =.0 Ng5cubic meter of eQecti+e reactor charcoal in+entory which is the charcoal bed +olume abo+e theoutlet collector assembly. nce the reagent has beentransferred to the drum" begin adding it to the circulating-mmonia water +ia the 8ductor ( J >= ).
The total reagent re/uired should be added at a uniformrate o+er a four to eight hour period.
;ote A The -mmonia water eYuent from the reactor outletshould remain colurless throughout the initial #erox catalyst impregnation procedure and this should be+eri'ed by periodically inspecting a sample of reactoroutlet -mmonia water for colour. &hould the -mmoniawater from the reactor become intensely blue in colour"there is reason to suspect channeling of the charcoalbed in which case the catalyst 9mpregnation should bestopped and steps underta!en to remo+e the bedchanneling. The channeling may be due to se+eral
reasons one being improper distribution by thedistributor pipe due to brea!arage etc."uring subse/uent catalyst reimpregnations" a bluecolour will appear in the -mmonia water coming from the reactor outlet. This is not unusual" since the old aged charcoal may no longer be able to absorb all of the #erox reagent. Particularly some of the moresoluble isomers. -s little as = PP# of #erox reagent issu*cient to gi+e a faint blue colour to the -mmoniawater. The following procedure must be used to remo+e
channels• bloc! in the reactor inlet " outlet lines.• 9n,ect a full amount of air for no longer than thirty
seconds to bubble or uQ the charcoal bed. "• if con+enient" somebody should obser+e at the
bubble patterns from the top manway. Largecoagulated bubbles would be an indication of
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channeling. - uniform bubble distribution would be an indication that channeling no longer exists.
?hen the drum is nearly empty of #erox reagent" ushit se+eral times with carrier solution and educt this intothe reactor in order to get all the residual recycle5cata6
lyst into the reactor. Continue circulation of ;$
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&uQ'cient caustic is to be in,ected to maintain a p$ inthe range of B to =% at the reactor drain pot outlet. Thecaustic in,ection pump P2=" P%= to be chec!ed fre/uentlyto assure that su*cient caustic is being pumped to the
reactors.
. The con+entional 'xed bed #erox reactor is nowprepared to recei+e some $C feed. uring continuousoperation of a con+entional 'xed bed or #erox =2 nit"the $C feed will gradually wash caustic out of thecharcoal bed. This caustic will collect in reactor waterdrain or interface pot. ?hen the caustic on the charcoalbecome depleted" mercaptan con+ersion +ia the #eroxreaction will cease to ta!e place. $owe+er" depletion isgradual" not sudden. - regular lab analysis program to
determine mercaptan sulfur in the product will show agradual increase in mercaptan concentration with time. This is largely caused by loss of al!alinity and itbecomes necessary to real!alinie the bed periodically. The amount of surface acti+e material presentA64oth naturally occurring sulfonates and naphthenates and synthetic corrosion inhibitor additi+es. i.e. if prewashing to remo+e ;aphthenates is ine*cientreal!aliniing of the bed must be done more fre/uently.
,.1.; INITIAL COMMISSIONING
P"!liina"4 In$8!3ion A 9nspection is the mostimportant step in start up preparation. -ll e/uipmentsmust be carefully inspected to see that it conforms inall respects to the detailed drawing and speci'cations.-ll respecti+e lines should be traced to see that theyconform to the detailed piping drawing andspeci'cations. -ttention should be gi+en to locations of +ents5drains5gauge glasses pressure gauges" sample points" pressure gauge" temperature indicator" relief +al+es to ensure that they are installed in accessiblelocations.Great attention must be gi+en to installation of trayspac!ing supports and internal distributors. etailed inspection criteria will be co+ered later along withspeci'c loading instructions.
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P"!$$&"! T!$ing ' -fter ascertaining by careful chec!that all internal e/uipment is properly installed and all+essels are clean and free of construction debris" +esselmanholes should be closed and the +essels and piping
should be pressure tested $ydraulically" using water inaccordance with the rating set forth in the pressurecerti'cate for the particular +essels. 4linds must beinstalld in suitable locations to isolate +essels ande/uipment which ha+e a lower pressure rating than the particular +essel or e/uipment being tested.sually the $ydraulic pressure test is carried out at =.>times the design pressure" but the proper test pressuresmust be ascertained for each +essel in /uestion.
6!"4 I8o"an ' -ll new pumps should be run forsu*cient time to properly wear in the pac!ing " so thatbearings will not o+erheat when the pumps are 'nallyplaced in ser+ice. 9n practice it is run for %0 hours"suction strainers should be in place during this timeand for the 'rst se+eral days after commencing actualoperation. This is for the protection of the pump fromany dirt or construction debris.
In$"&!n$ ' These must be carefully chec!ed forcorrect installation and calibration by a /uali'ed instrument personnel. -ll tests that can be performedto simulate actual operating conditions should be carriedout to ensure that the instrument will operate properly.-ll ori'ce plates should be chec!ed to see that theyconform to the speci'cations.
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CHAPTER ;
NORMAL STARTUP
4efore the feed is ta!en into the unit" it is necessary to expel air from all e/uipments and pipelines" as it is apotential 're haard.
-ir elimination can be done by ;itrogen purging.8ntire system is lined up and air elimination done by ;itrogenpurging.
M!"o0 R!a3o" ) R >1 +
7eactor should be ;% purged to an xygen content of less than >X by lining up ;% through 7eactor +ent line.7eactor inlet " outlet +al+es to be closed and drain pot exit+al+e (i5+ u5s of L:22=) to be closed..8nsure all the drains and +ents are closed.;itrogen Purging should be carried out byPressurising the reactor with ;% to approx =>6%2 Psig.epressurising to atmospheric pressure.-gain pressurising the reactor to => 6 %2 Psig.with ;% and again depressurising it to atmospheric pressure. Thismethod of pressuriation and depressurisation should be
repeated until the oxygen content is less than > +olX.7eactor to be pressurised with FG by opening the feed inlet+al+e of the reactor.;ow the system is ready for recei+ing Gasoline.
S!8$ &n#!"a!n o8!"aion a"! RChec! with blending people ( 7TF) whether the designated tan! is ready to recei+e the product. Then open the 45L +al+es. 9nform FCC of starting the treatment of Gasoline.?hen Gasoline product from FCC is con'rmed to speci'edproperties" route Gasoline to #erox nit.
Caustic in,ection pumps P2=- and P%= to be started andcaustic in,ection to be started at the maximum rate..Gasoline ow through the unit is lined up as followsA
Gasoline feed 6666 Gasoline feed cooler &>% 666 $: 2=> 66667eactor(7 2=) 666esignated Tan! or slop tan!.Gasoline feed 6666 Gasoline feed cooler &>
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The #erox reactors are 'lled with Gasoline completely andthis is ascertained by o+erow in +ent line.?nem the reactor is full of hydrocarbon" reactor pressure tobe increased to operating pressure with the bac!pressurecontroller.
9nform Nerosene #erox for want of air" open the air owindicating controller ( F9C 2=1 ) to 72= and F9C 2=D to 7%= toa desired amount and switch o+er to automatic operation.?hen a/ueous eQuluent apperas at the reactor water drainor interface pot" the interface le+el controller (L9C 22=) to becommissioned and the caustic in,ection rate in increments toobtain B6=% p$ drain eQulent.&tart the #erox plus in,ection pump ( P 2% - and P%%) toin,ect #erox plus acti+ator into the untreated Gasoline line.
The system pressure controlled at Ng5cm%g by P9C22= for 72= and by P9C 22% for 7%=..
&le product for doctor test. 9f negati+e" treatedproduct can be sent to storage tan! .
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CHAPTER <
NORMAL SHUT DOWN
sually normal shutdown ta!es place to carryoutscheduled turn around for maintenance ,obs.
ust before shut down" inform 7TF to switch o+er Gasoline rundown as there will be no more sweetening and con'rm" that Gasoline rundown switched o+er to someother tan!.
Cut oQ air in,ection to 72= reactor by closing F: 2=1 andto 7%= by closing F:2=D. 9nform Nerosene #erox about the
shutdown.i+ert Gasoline ow to slop tan!. 4loc! oQ Gasoline#erox battery limit :al+e. epressure #erox nit throughbac! pressure control. Then pump out through P >= - toslop tan!.
&top caustic in,ection pump (P 2= - and P%=) to cut oQ in caustic in,ection.
&top #erox plus in,ection pump P 2%- and P%% to cut oQ the in,ection of catalyst acti+ated.
Complete isolation must be attained between feed stoc! line and in,ection lines of air and caustic soda by closing
each isolation +al+es located upstream of in,ection points.
=
-)" 8ach +essel must be under a slight pressure to a+oidpulling a +acuum. This can be done by a small owstream of ;itrogen through the following +essels.
7 2= 6 #erox reactor 7%= 6 #erox 7eactor
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N.B A Permanent steam connection is pro+ided for the following +essels A
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CHAPTER ?
EMERGENCY SHUT DOWN
PROCEDURES
-n emergency shut down warranted if on or morecombinations of the following occurs.
FCC upset5feed failure.Power Failure9nstrument -ir Failure&team Failure.
For all the abo+e" the unit can be temporarily isolated" until the failed ser+ice is brought bac! to normal condition" can then be restarted simply by opening the isolation +al+e. 9t should borne in mind to protect the product tan!s" ascontamination should be a+oided.
(=) (CCU (ail&"!
4ypass Gasoline #erox and route the Gasoline to slopimmediately" to a+oid oQ spec. Gasoline from coming incontact and contaminating the #erox reactor beds. 7eturn the unit to ser+ice once upset is corrected and Gasolineresults are o!.For the abo+e close 4 5 L isolation +al+e on the Gasoline feedline and P9C 22= on treated Gasoline line. Cut oQ airin,ection by closing the @: 22= E F9C 2=1. &imilarly cut oQ airin,ection by closing the @: 22% and F9C 2=D. 9solate Gasolinefeed and Close P9C 22% on treated Gasoline line.&top the following pumps and close the discharge +al+es
P 2= - and P%= caustic circulation pump P 2% - and P%% #erox Plus in,ection pump
)2+ Pow!" (ail&"!
Gasoline feed pump" caustic in,ection and #erox plusin,ection cease functioning. 4y pass the unit as abo+e and
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bottle up. -s power is reco+ered restart pumps and return tonormal operation.
)+ In$"&!n Ai" (ail&"!
9n case of instruments air failure happens" all control+al+es go to fail safe position. This results in all control +al+es in the unit to shut down and isolate the unit. List of instruments on FC5F are gi+en at the end of the manual.4ypass unit until air is restored. -lso close caustic in,ection"#erox plus in,ection pumps.
),+ S!a (ail&"!
8+en though no steam is used in Gasoline #erox in normal operation" steam failure will aQect the FCC. There
is a danger that oQ spec. Gasoline may come to #erox nit.4y pass #erox unit and bottle up until Gasoline comes on spec. Neep 7TF informed of the situation and con'rm thatGasoline is switched o+er. nce Gasoline comes on specinform to 7TF to switch to product tan!s.
CHAPTER 12
SPECIAL PROCEDURES
REACTOR BED HOT WATER WASHING
?hen ad,ustment of the operating +ariables is nolonger su*cient to maintain catalyst bed acti+ity" thecharcoal bed can be hot water washed to remo+e sundryorganic compounds and caustic neutraliation soaps whichha+e deposited in the charcoal pores or otherwise physically
bloc!ed oQ the acti+e catalyst surface. &ince many of these compounds are water soluble" catalyst bed acti+ity will be restored when they are ushed from the charcoal. $ot waterwashing is also necessary to remo+e sodium soaps andal!alinity from the charcoal prior to catalyst reimpregnation. The phenomenon of charcoal pore plugging or coating is gradual and" hence" allows the bed washing to be scheduledwith minimum incon+enience to general re'ning operations
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and scheduling. $ot water washing may also be eQecti+e in reducing or eliminating reactor bed pressure drop whichshould ne+er be allowed to exceed 2. Ng. The water usedfor reactor washing should be either clean steamcondensate or deionied water that is free of dirt"
suspended matter" hardness" excessi+e salts" and acti+echlorine as in hypochlorite. The washing procedure is as follows
&top the air in,ection and hydrocarbon ow to the reactor. Pro+ision should be made to pump 6 or pressure 6 out allhydrocarbon from the #erox reactor under steam or nitrogenpressure.1. Fill the reactor with warm" >23C warm water. This should
be done by passing Cold Condensate through J >% andopening LP steam after 'lling half of the +essel stopwater. Pump this wash water to spent caustic facilities.
7epeat this procedure. This step will greatly reduce theal!alinity of the wash water discharged to the sewer system and will also protect the +essel from causticattac!.
2. -fter the hydrocarbon has been pumped from thereactor and the ma,or portion of the residual caustic hasbeen remo+ed" begin steam in,ection downow throughthe bed +ia the water heater in the reactor. 9t will ta!eapproximately one or two hours for this step to remo+e most of the remaining hydrocarbon from high aromatic feedstoc!s. The reactor drain eYuent is usually cooled
for safety using direct cold water /uench of an eYuent heat exchanger.
3. Commission the water heater and introduce hot" %22 6%=23F" (B> 6 BB3) water +ia the reactor inlet distributor ata rate of approximately 2.1> #
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5. 9f the bed is being washed solely to reacti+ate thecatalyst by cleaning the charcoal pores" the washing iscompleted when the wash water is clean and essentially colourless. 9f the bed is being water washed prior to acatalyst reimpregnation" hot water washing is continued
until the eYuent water p$ is reduced to between D and B. This will minimie acetic acid consumption in a later step.6. Gradually stop the steam ow" but continue to introduce
cool condensate through the water heater into the reactor to cool the heater into the reactor to cool the charcoal bed down to a temperature of about =023F (123C).;itrogen can be used to maintain the reactor under slight positi+e pressure.
7. -fter the bed is cooled" the water is displaced with nitrogen pressure and all of the water in the reactor isdrained.
8. For a con+entional 'xed bed #erox nit" the catalyst bedmust be al!alinied with fresh caustic (%23 to
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function of proper operation $C and mercaptan types" crudesource" feed impurities etc and may +ary from < months toa year or e+en longer" when re/uired the catalystreimpregnation is to be done.
P"o3!#&"! '
1. The washing procedure has to be followed from steps = to. ?hen eYuent water p$ is reduced to D to B or to a p$which no longer seems to be dropping" stop washing"while washing the reactor bed also ush out the circulationpump suction and discharge lines to remo+e any residualal!alinity with slight positi+e pressure on the reactor.Please note that the water drained after acidi'cation iscolored. This indicates the acid addition was eQecti+e inreleasing additional contamination from the catalyst
bed. &top circulation when the le+el is below distributor pipe. -pproximately %2 #
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3. Place about %D lt of -cetic acid in to the acetic acidaddition pot pro+ided. The acetic acid can be placed in the drum used for catalyst impregnation or a rubberhose can be put directly into the -cetic -cid container.8duct the acid into the circulating water by regulating the
globe +al+e in the line from pump discharge into thesuction of the eductor. The glacial -cetic -cid should beadded to the system o+er a period of >6=2 minutes.
Note : %D lts per reactor of commercial grade glacial acetic acid re/uired -cetic -cid is not re/uired for the initialimpregnation of reactor. 9t is needed only for subse/uent7eimpregnation.
4. -fter circulating the acidi'ed water for one hour" chec!the water p$ at the sample point in the circulation pump
suction line. 9f the circulating water p$ exceeds 1.>" eductanother about %2 lt of -cetic -cid" as described abo+e.-fter another hour" again chec! p$ of water from thereactor outlet. continue this procedure until the water p$is 1.> or less. This pro+ides on the bed slight acidicmedium.
5. rain the acidi'ed water from the reactor drain usingnitrogen to maintain a slight positi+e pressure on thereactor. ;ote that the water drained after acidi'cation iscolouredR this is an indication that acid addition waseQecti+e in releasing additional contaminants from the
catalyst bed.6. nce the bed is drained the reimpregnation is done as
disscussed in the impregnaiton procedure.
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CHAPTER 1,
TROUBLE SHOOTING
The failure in mercaptan sweetening in the #erox inletcan be attributed to one or more or combination of thefollowingR
a) Lac! of caustic b) 9nsu*cient -ir c) 7eactor channeling d) #echanical interference with the catalyst
e) Loss of catalytic acti+ity f) 8mulsi'cation and caustic entrainment.
)a+ La3 o Ca&$i3 '
The presence of caustic is essential in the #erox7eactor. ?hen the &odium $ydroxide is either consumed out or wea!ened out" #ercaptan oxidation will no longerproceed. This is e+ident by the increase in mercaptan sulfur
content in the treated Gasoline. $ence resaturation of thecatalyst bed must be carried out to restore the sweetening process. se of %2 34e fresh caustic is ad+ised. nly byoperating experience fre/uency of saturation can be determined. $owe+er a mere fre/uent caustic wash willensure su*cient al!alinity.
&ul'des may seriously impede caustic regenerationdue to oxidation of sul'de ion in preference to mercaptideion.
H2S - 2NaOH Na2S - 2H2O.
$ence the source of hydrogen sul'de must be eliminated.?hen all of the sul'de is oxidied" the catalyst will againbegin to oxidie mercaptan. 7aising the catalyst concentra6tion" caustic temperature and air rate may be used to speed
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up elimination of sul'de interference. $ence two batch type caustic prewasgh is employed in series. This will allow greater utilisation of caustic without ris!ing $%& lea!ageinto #erox nit.
p to a certain point the presence of acid oilsimpro+es extraction. ?hen their presence interferes withcaustic ow in the extractor caustic entrainment may ta!eplace. -ccumulation of regenerated acidic materialsmay consume casutic" by C% pic!ed up from theregeneration air. nly experience can determine the extent to whcih spending the caustic with wea! acid can betolerated before extracting e*ciently drop oQ.
)%+ In$&3i!n Ai"
This often happens when there is an increase inmercaptan sulfur" or the total Gasoline treated through thisunit. -ir in,ection rate must be ad,usted. -ccordingly toaccomodate these changes in air concentration is generally !ept at =>2 6 %22X of stoichiometric re/uirement"higher conentration is possible as long as all the air isdissol+ed. xidation reactions other than that of mercaptans will be promoted at higher concentration andthis must be considered when using a higher in,ection rate.
9f insu*cient air is suspected chec! the reactors
pressure to ma!e sure all air is dissol+ed. Chec! the air ow meter to see if air is going in at the right rate. &ubmit Gasoline samples to analyse the mercaptans load and see if there is any change. -d,ust air rate accordingly.
)3+ R!a3o" Cann!lling
?hen the catalyst is new or !nown to ha+e lost acti+ityand when it has been determined that ade/uate air is
present" channeling should be suspected. - separate airphase will almost always induce channelling. -d,ust systempressure to dissol+e the in,ected air. Channelling can thenbe corrected by fu*ng the bed with air or nitrogen for
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The acti+ated charcoal bed absorbs ;aphthenic acids"trace compounds such as high molecular weight$ydrocarbon" particulates and ;itrogen compounds.-ccumulation of these materials will plug catalyst pores and
plug up acti+e sites thus reducing the acti+ity of the catalyst. This is e+ident by obser+ing the increasing pressure drop across the reactor. The catalyst acti+ity can be partiallyreco+ered by hot water washing the reactor bed. 9f waterwashing is ineQecti+e" the charcoal bed must beimpregnated.
)!+ Lo$$ o Caal4i3 A3ii4
9t is normal for the #erox catalyst to gradually lose its
eQecti+eness" as the unit ages. The treated Gasoline becomes more concentrated in mercaptan sulfur and doesnot produce speci'cation product. 9t is necessary to causticwash the reactor more fre/uently and more concentratedcaustic solution is to be used. ther means to help the #erox reaction are to increase reactor temperature and theoxygen content e+entually mercaptan re/uirement can nolonger be made despite continuous saturation"reimpregnation will be re/uired.
)+ E&l$i73aion an# Ca&$i3 En"ain!n
#erox catalyst in caustic solution does not increasethe tendency of caustic solution to emulsify with $ydrocar6bons. 9t does howe+er" increase the detergent properties of caustic.
&cale and dirt will be almost completelydislodged5absorbed by #erox catalyst.
Finely diluted suspended material can stabilise emul6sions. 9t may be necessary to discard the 'rst batch of
caustic if it pic!s up a big load of scale and dirt from usede/uipment.
Part of this scale and dirt may be iron sul'de. 9tappears that preferential oxidation of such sul'de maypre+ent the catalyst from promoting oxidation of mercap6tan.
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CHAPTER 1
LIST O( SPECIAL E@UIPMENT
1. &pecial chec! +al+e J %=2. 8ductor J >=3. -ir #ixer J %%4. &pray ;oles J 2
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9nlet Temperature A , +
&er+ice A #ixing of -ir and
$ydrocarbon
-ir Pipe &ie A =
Tee &ie A 1
#C A Carbon &teel" except && 'lter
element
) , + S8"a4 NoJJl!$ ) Y >K Y2 +&er+ice A For Caustic in,ection to thehydrocarbon Type A 7emo+able in,ection noleassembly
#C A % T 5 h Turndown A > to =#ax. Temp. A % !g5cm%g
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Temp. A = oC-llowalbe temp. A == oC :ariation
D!$&8!"!a!" Wa!" Temp. A 12 oCFlow 7ate A 2.== m
LABORATORY RE@UIREMENT
SCHEDULE
The ultimate ob,ecti+e of petroleum re'ning is to produce
product hydrocarbon streams which meet all speci'cations re/uired for
their ultimate end use. To accomplish this ob,ecti+e" it becomes
necessary to characterie the important physical and chemical
properties of the +arious re'nery streams utiliing speci'c laboratory
analytical testing procedures. Thus" satisfactory re'nery operation
depends largely upon proper analytical procedures for /uality control.
The sample point should be well purged to eliminate aged
material" water" dirt" etc." and assure withdrawal of sample
representati+e of the material in the pipe at that point in time. The
sample container must be ade/uate for the analysis to be obtained.
nce a proper sample has been obtained" it must be preser+ed
intact until analyed. This re/uire the preser+ation of itUs physical and
chemical changes in the sample.
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1>.1 SCHEDULES AND TEST METHODS
&uggested analytical schedule for the Gasoline #erox unit is
gi+en below. These represent a minimum recommendation for an
ad/uate /uality control program.
&.;. &T78-# ;-#8 E T8&T
;-#8
T8&T #8T$ F78H8;CJ
= Gasoline Feed
• istillation
• $ydrogen sul'de
• #ercaptan &ulfur
• Particulates
• Gra+ity
-&T# D1
P =1<
P =1<
-&T# %%1
-&T# =%BD
nce in a day
I
I
?ee!ly
aily
•
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% Fixed bed reactor inlet
• iagnostic
< • rain Pot eYuent
• P$
• Total -l!alinity
• Gra+ity
• -cid oils
P
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• ctane ;umber
• xygen Content
• :C
• Toxics 7eduction
• ;ox reduction
• 8xistent Gum
-&T# %1BB and %22
8P- formula
8P- formula
8P- formula
-&T#
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;oteA
The sampling and analysis same for 7eactor ;o.%.
CHAPTER 15
SA(ETY
-ll the rules of safety in the re'nery operation apply to the operation of
the #erox Process. -ll employees and persons responsible for
operation of the #erox process should be familiar with applicable
safety practices. -ll necessary precautions should be ta!en to a+oid
accidents.
15.1 INTERNAL (IRE
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The presence of air and hydrocarbons in #erox Process
e/uipment" particularly the excess air +ent line" is not considered to be
any more haardous than other situations in re'neries in which air and
hydrocarbons +apors exist.
Locations of &afety shower
=. ;orth of #T67F0=162= (Caustic &torage tan!)
%. &outh of #T67F0=162%
Ma!"ial Sa!4 Daa S!! o" Ca&$i3 '
Properties and characteristicsA
Physical state A Turbid solution
Colour A ?ater white to slightly coloured
?ater solubility A Complete
#olecular weight A 02.2=
Flash point A ;on ammable
#ode of entrance into body A 9nhalation" ingestion and contact
7eacti+ity A
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The solution is stable in nature and
haardous. 9t is slowly corrosi+e to iron and copper. 7eacts +iolently
with many organic chemicals such as acrolein" acrylonitrile" alcohols"
chloroform" malei anhydride etc
$ealth $aards A
9n,ury may result before one realies that
chemical is in contact. 9t is toxic and damages tissures.
9nhalation A 9n,ury to entire respiratory tract.
Prolonged exposure may lead to inammation of lungs.
&!in A estruction of tissues" burns and
ulcerations.
8yes A &e+ere damage and may lead to
con,uncti+itis" corneal burn etc.
9ngestion A &e+ere burns of the mucous
membranes of the mouth" throat"esophagus and stomach.
Perforation of tissue may follow.
Fire and 8xplosion $aards A 9nstances of +iolent decomposition of
organic materials ha+e been recorded
following usuage of caustic soda solution
for cleaning production e/uipment.
Contact with water or moisture may
generate su*cient heat to ignite
combustible material.
$andling and &torage A For protection of
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=. 7espiration 6 Filters respirators
%. $ands 6 :inyl or neoprene
glo+es
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&!in contact A 8mergency shower bath" followed by
remo+al of clothing while still under the
shower. &ee the physician.
8ye contact A 9rrigate for at least => minutes. Neep
eye lids apart and mo+e eyes in all
directions and ha+e irrigation continued.
9ngestion A rin! lot of water5mil!. onUt induce
+omiting unless ad+ised by physician.
=X acetic acid solution can be gi+en.
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CHAPTER 1;
CHEMICAL CONSUMPTION
1;.1 CHEMICAL CONSUMPTION
=. P #erox D catalyst 00 m.Ltrs 5 hr E
#aximum .0 Ltrs5h. continuously to the reactorcharge.
3. -cetic -cid 6 %D Litres5reactorCommercial grade glacial acetic acid is used.;ot re/uired for initial impregnation but re/uiredfor further reimpregnation.
4. -mmonia 6 =%0 Ng5reactorLi/uid anhydrous ammonia in cylinders is used.
5. Caustic =234e 6 1D #
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CHAPTER 11
E@UIPMENT DETAILS
S.NO TAG NO E@PT.
TITLE
DESIGN OPERATING ID MM CO
M
T8#P
8G C
P78&&
NG5C#%G
T8#P
8G C
P78&&
NG5C#%G
= #: 7F0=1:2=
78-CT7;. =
2 =D.
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6ESSEL DETAILS
S.NO. TAG NO E@PT TITLE DESIGN OPERATING
M
TEMP
DEG C
PRESS
*GCM2G
TEMP
DEG C
PRESS
*GCM2G= #: 7F0=16
:2%
7-9; PT 2 =D. =
9;$949T7
9;8CT9;
T-;N
2 X of ;ominal tan! capacity.
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61 66
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PRESSURE RELIE( 6AL6ES
S.
NO
TAG
NO
SER6ICE SET PR
*GCM2G
PRESS *GCM2G TEMP DEG C BAS
SE
NORMAL MA= NORM MA== =2=- 7eactor =
+ent
=.> >.1 =D. >.1 =D.
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S.
NO
TAG
NO
SER6ICE SET PR
*GCM2G
PRESS *GCM2G
NORMAL MA=
TEMP DEG C
NORMAL MA=
BAS
SE
== =>=- Nero =
Caustic in,.
Pump -
%0.1 =0 %0.1 =4 Nero =
Caustic in,.
Pump 4
%0.1 =0 %0.1 % Nero %
Caustic in,.
Pump
%0.1 =0 %0.1 < -ir mixer out
to 7eactor =
=.B >. =>0 -ir mixer out
to 7eactor %
=.B >. = &$8LL Gasoline %.0< C& ==% .20 C& =2%
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wash
eQuluent T48 C? C& =-54 -mmoniate
d water
=.2> =.2> >.% 1.<
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P< < o 4e
Caustic
2.> 2.2 =1 =
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