MEROX OPERATING MANUAL INDEX S. No. 1 2 DESCRIPTION Page No.

INTRODUCTION MEROX PROCESS DESCRIPTION MEROX PROCESS EQUIPMENT PRETREATMENT EXTRACTION SECTION SWEETENING POST TREATMENT MEROX CATALYSTS U-21 ATF /S MEROX UNIT CAPACITY FEED SPECIFICATIONS PRODUCT SPECIFICATIONS TYPE OF CATALYST USED PROCESS DESCRIPTION DETAILED DESCRIPTION OF P!ID PRE-COMMISSIONING OPERATION STARTUP PROCEDURE REACTOR "ED WATER WAS#ING AND REIMPREGNATION S#UTDOWN PROCEDURE EMERGENCIES OPERATING $ARIA"LES C#EMICALS AND CATALYSTS MODIFICATIONS U-22 STRAIG#T RUN LPG MEROX UNIT CAPACITY FEED SPECIFICATIONS PRODUCT SPECIFICATIONS PROCESS DESCRIPTION DETAILED DESCRIPTION OF P!ID PRE-COMMISSIONING OPERATION STARTUP PROCEDURE S#UTDOWN PROCEDURE EMERGENCIES OPERATING $ARIA"LES C#EMICALS AND CATALYSTS MODIFICATIONS

-1-

-2-

S. No. &

DESCRIPTION Page No. U-23 $"N MEROX UNIT CAPACITY FEED SPECIFICATIONS PRODUCT SPECIFICATIONS TYPE OF CATALYST USED PROCESS DESCRIPTION DETAILED DESCRIPTION OF P!ID PRE-COMMISSIONING OPERATION STARTUP PROCEDURE REACTOR "ED WATER WAS#ING AND REIMPREGNATION S#UTDOWN PROCEDURE EMERGENCIES OPERATING $ARIA"LES C#EMICALS AND CATALYSTS U-2% CRAC ED LPG MEROX UNIT CAPACITY FEED SPECIFICATIONS PRODUCT SPECIFICATIONS TYPE OF CATALYST USED PROCESS DESCRIPTION DETAILED DESCRIPTION OF P!ID PRE-COMMISSIONING OPERATION STARTUP PROCEDURE S#UTDOWN PROCEDURE EMERGENCIES OPERATING $ARIA"LES TROU"LE S#OOTING U-2& CRAC ED FCCG MEROX UNIT CAPACITY FEED SPECIFICATIONS PRODUCT SPECIFICATIONS PROCESS DESCRIPTION DETAILED DESCRIPTION OF P!ID PRE-COMMISSIONING OPERATION STARTUP PROCEDURE S#UTDOWN PROCEDURE EMERGENCIES OPERATING $ARIA"LES MODIFICATIONS SAFETY ! FIRE FIG#TING FACILITIES
-3-

1. INTRODUCTION' Straight-run LPG, gasoline and kerosene fractions obtained from atmospheric distillation may contain hydrogen sulphide and mercaptans. the e tent of !hich mainly depends upon the type of crude processed. Similar products from secondary processes such as "## also contain hydrogen sulphide and mercaptans to a greater degree compared to straight-run products. $ydrogen sulphide is corrosi%e and should be remo%e in order to meet specifications on corrosion rate. &he specification for LPG, gasolene, 'erosene and (&" include copper strip corrosion test !hich is a measure of rate of corrosion on copper containing materials.)ercaptans are substances !ith obno ious odour and, therefore, in order to handle and store them, mercaptan le%el !ill ha%e to be brought do!n to a acceptable odour le%el. &he specifications of abo%e products include *+octor &est* !hich must be negati%e and is generally related to the e tent of mercaptan present. $ydrogen-sulphide can be easily remo%ed by !ashing !ith dilute caustic solution. $o!e%er, for reducing the mercaptans le%el many processes are a%ailable like, Strong alkali-!ash #opper s!eetening +octor s!eetening )ero process $ydrodesulphurisation (lkali-!ash is effecti%e only if lo! molecular !eight mercaptans are in%ol%ed. $ydrodesulphurisation is normally employed only if reduction of total sulphur le%el is also re-uired. .oth in%estment and operating costs are higher in case of hydrodesulphurisation. /ut of other proceses a%ailable, )ero process is considered a superior and pro%en process.

-4-

2. MEROX PROCESS DESCRIPTION &he )ero process licensed by )0S 1ni%ersal /il Products #o., 21/P3, 1S(, is for the chemical treatment of LPG, gasolene and distillates to remo%e mercaptans into disulphides. &he remo%al of mercaptans may be either partial or full. &he chemical treatment is based on the ability of )ero catalysts to promote the o idation of mercaptan to disulphide using air as the source of o ygen. &he o%erall reaction is as follo!s, 45S$ 6 704/4 -8 5SS5 6 $4/ &he o idation is carried out in the presence of an a-ueous alkaline solution such as either sodium hydro ide or potassium hydro ide. &he reaction proceeds at an economical rate at normal rundo!n temperature of refinery streams. Lo! molecular !eight mercaptans are soluble in caustic solution and therefore !hen treating LPG and light gasoline fractions, the process can be used to e tract mercaptan to the e tent, they are soluble in caustic. 9 traction of mercaptan reduces the sulphur content of the treated product. (lternati%ely mercaptans can be con%erted to disulphides !ithout remo%ing any sulphur from the treated stock in !hich case the operation is referred to as s!eetening. :n the treatment of hea%ier boiling fractions such as hea%y naphtha and kerosene only s!eetening is possible. MEROX PROCESS EQUIPMENT'

:n order to understand the function of %arious )ero process e-uipment. the e-uipment can be broadly di%ided into follo!ing sections , Pretreatment for remo%al of hydrogen sulphide and naphthenic acids, if present. &he method %aries !ith properties and conditions of feedstock and in some cases may not be re-uired. 9 traction section !here re-uired, for remo%al of caustic soluble mercaptans and thus reduce sulphur in the treated product. S!eetening for con%ersion of mercaptans to disulphides. "or a gi%en capacity plant, the )ero reactor si;e can %ary depending on the case of s!eetening due to the type of mercaptans present and also on product re-uirement. Post-treatment to remo%e caustic ha;e and to control properties not affected by )ero process. $ence post-treatment needed depends on products, utilisation and type of contaminants present in the feedstock. &aking each section in turn, function of each e-uipment can be described. PRETREATMENT

Petroleum fractions may contain hydrogen sulphide and stocks boiling higher than 78<=# may also contain naphthenic acids. $ydrogen sulphide is not a catalyst poison as such, but !ill dilute the caustic containing )ero catalyst by reacting
-5-

!ith caustic. "urther it blocks some of the catalyst acti%ity sites slo!ing do!n the normal reaction and also consumes part of the o ygen a%ailable. $ence, it is recommended that hydrogen sulphide is remo%ed by !ashing !ith dilute alkali solution before the distillate is sent to reactor for treatment. >aphthenic acids also interfere !ith treating operations and must be remo%ed prior to treatment. &he reactor contains caustic and if naphthenic acids are not remo%e they form sodium naphthenates !hich coat the catalyst and block the pores. "or remo%al of napthenic acids, the procedure used is to !ash !ith dilute caustic. +ilute caustic is used so as to a%oid formation of emulsions. &here could, ho!e%er, be some carry-o%er of ha;e depending on the acidity of stock treated. &he ha;e can easily be remo%ed by coalescing through a sand filter. "eedstocks, !here carry-o%er of !ater from distillation units can be e pected must be passed through a coalescer for remo%al of suspended !ater prior to caustic !ash, !hich !ould other!ise dilute the caustic used for pretreatment. EXTRACTION SECTION

(s pre%iously stated, lo! molecular !eight marcaptans are caustic soluble and can easily be remo%ed by !ashing !ith caustic in a counter current to!er. :mpro%ed e traction is fa%ored by, Lo! temperature. $igh concentration of caustic. Lo!er molecular !t. of mercaptans &ype of mercaptans, %i;. normal mercaptans are easily e tractable, tertiary mercaptans least e tractable and secondary being in bet!een. &he mercaptan enters the caustic solution and reacts as follo!s, 5S$ 6 >a/$ ?-8 >aS5 6 $4/ &his is being a re%ersible reaction the degree of completion of reaction is go%erned by normal e-uilibrium la!s. &he sodium mercaptide is readily o idised to disulphide in the presence of )ero catalyst as sho!n , 4>aS5 6 l04/4 6 $4/ -8 4>a/$ 6 5SS5 &his is not a re%ersible reaction and the reaction rate is speeded up by, 5aising the temperature. 1se of e cess air. :ncreasing the intimacy of contact.
-6-

:ncreasing the catalyst concentration. &he o idation of mercaptides is carried out in o idiser in the presence of mero catalyst. &he disulfides oil, !hich is formed, separates out from caustic as it is insoluble in caustic. #austic can be reused for e traction. &he presence of )ero catalyst in e traction caustic does not ho!e%er, affect the amount of mercaptans e tracted. and e traction is dependent only on parameters e plained earlier . SWEETENING

S!eetening can be defined as con%ersion of mercaptan sulphur present in a hydrocarbon stream to disulphide sulphur !ithout actually reducing sulphur content of treated stock. &he s!eetening process is based on the ability of )ero catalyst to promote the o idation of mercaptans to disulphides using air as the source of o ygen. &he reaction is as follo!s, 5S$ 6 >a/$ ?-8 >aS5 6 $4/ 4>aS5 6 l04/4 6 $4/ -8 4>a/$ 6 5SS5 (s can be seen from reactions, the o idation is carried out only in the presence of alkali solution. &he S!eetening can be accomplished either in solid bed s!eetening, !here the hydrocarbons and caustic are simultaneously controlled o%er a solid support impregnated !ith )ero catalyst. Li-uid-li-uid s!eetening !here hydrocarbon, air and caustic containing )ero catalyst, air simultaneously controlled in a mi er. Solid bed s!eetening consists of a reactor, !hich contains a bed of acti%ated charcoal impregnated !ith )ero catalyst and kept !et !ith caustic solution. :mpregnation of catalyst on bed is achie%ed by dissol%ing the catalyst !ith ammonia solution and pumping ammonia solution o%er charcoal. (ir is in@ected ahead of reactor and in the presence of mero catalyst the mercaptans are o idised to disulphides. &he reactor is follo!ed by a settler !hich ser%es as reser%oir of caustic. #austic is intermittently circulated from the settler o%er the catalyst bed to !et the charcoal. "or li-uid-li-uid s!eetening, the most common type of mi er used is the orifice plate mi er, !hich is a %essel, fitted !ith a series of plates !ith orifices. &he %essel pro%ides ade-uate residence time and the orifice plates create enough turbulence to bring about the intimate contact bet!een hydrocarbon, caustic, catalyst and air. &he problem of accomplishing li-uid-li-uid s!eetening is one of getting the difficulty soluble mercaptans into the caustic phase for sufficient time to permit their o idation. &he higher the molecular !eight or the more highly branched the mercaptan is, the more difficult it is to accomplish necessary mi ing. $ence hea%y gasoline and 'erosene may ha%e to be treated using fi ed bed reactor.

-7-

POST TREATMENT

&he product from the mero reactor !ill at times contain caustic ha;e. Post treatment is re-uired if the product is to go to storage, clear and bright. :n most cases pro%ision of caustic settler and sand filter is ade-uate to remo%e caustic ha;e. $o!e%er, for treatment of (&", !hich has to meet stringent specification caustic must be remo%ed by !ater !ash after caustic settling. Aater !ash remo%es entrained caustic as !ell as !ater soluble surfactants, Aater !ash is follo!ed by a salt filter to remo%e entrained !ater and part of the dissol%ed !ater. &his may be follo!ed by clay filter to remo%e copper and !ater insoluble surfactants, if present in feed. MEROX CATALYSTS'

&here are t!o types of )ero catalyst, each one being used for specific ser%ice. #atalyst ". is to be used on units e-uipped !ith solid bed s!eetening reactors. #atalyst AS is used for li-uid-li-uid s!eetening in mi ers. &his is a caustic dispersible catalyst. &his is also used for o idation of e traction caustic in o idisers.

-8-

3. U-21 ATF /S

MEROX '

UNIT CAPACITY'

&he )ero 1nit for treating kerosene B (&" streams from the (tmospheric +istillation unit has been designed to feed 7.C million metric tons per year of kerosene !hile processing a C<, C< mi ture of Light (rabian, >orth 5umalia crudes. &he 1nit shall operate for DEC stream days in a year. FEED SPECIFICATIONS'

&he kerosene to be treated in the )ero 1nit shall ha%e substantially the follo!ing properties, 2i3 2ii3 2iii3 2i%3 2%3 2%i3 2%ii3 .oiling 5ange :.P0".P o# Specific gra%ity at 7C.6=# &otal acidity, )g 'o$0Gm )ercaptan Sulphur !t ppm &otal Sulphur !t.G. $4S !t ppm #olour, Saybolt 7E<-47< )a . <.7FC to <.84 <.<4 7C< <.44 7< ma 6 D<

PRODUCT SPECIFICATIONS' treatment shall meet the follo!ing

&he Product kerosene0(&" after )ero specifications, 2i3 (ppearance

Hisually, clear, bright and free from solid matter and undissol%ed !ater at normal ambient temperature. >o 7 )a imum >o < )a imum 7<-4< ppm 2ma .3 >egati%e C )a imum !hen feed stock is 4C min., pro%ided that the feed stock comes directly from the fractionation facility.
-9-

2ii3 2iii3 2i%3 2%3 2%i3

#orrosion copper strip #orrosion sil%er strip )ercaptan sulphur !t ppm +octor test #olour loss, saybolt

2%ii3

&hermal stability, 2a3 "ilter pressure drop in mm $g. 2b3 &ube 5ating %isual Aater separameter inde (cidity, mg. '/$0Gm 2a3 Aater Separometer inde 2modified3 2b3 A(&95 59(#&:/> :nterface 5ating Holume #hange #onducti%ity 2(&"3

4C.< ma imum Less than code D F< minimum <.<74 ma imum F< minimum 7.< ma imum 7.< ma imum C<-EC< psm

2%iii3 2i 3

2 3

I$4S free fresh stock chargeI shall mean fresh stock charge containing no $ 4S or if the fresh stock charge contains $ 4S, it shall be scrubbed out !ith caustic soda solution or sodium carbonate solution in the laboratory !ithout e posure to o ygen. TYPE OF CATALYST USED'

#atalyst used for s!eetening kerosene0(&" Stream in this treating unit is mero catalyst ". !hich is supplied by the 1ni%ersal /il-Products #ompany. &his catalyst is used in the t!o s!eetening 5eactors <47 57 ( and .. &he catalyst is impregnated on acti%ated charcoal beds in the reactors. Juantity of catalyst re-uired for one impregnation in the reactors is 4C< 'g. of acti%e ingredient. &he catalyst is supplied in li-uid from each 1S gallon containing 7 kg. of acti%e ingredient. PROCESS DESCRIPTION

Pretreatment for kero0(&" consists of a coalescer and caustic pre!ash %essel, for remo%al of suspended !ater and hydrogen sulphide, >aphthenic acid etc. S!eetening is achie%ed in supported catalyst bed reactor. &!o reactors in parallel ha%e been pro%ided. (ir re-uirement of all )ero units is supplied from a common compressor. (lso, storage tanks for receipt, dilution and storage of caustic and storage for methanol ha%e been pro%ided. Post treatment for kero0(&" consists of caustic settling. !ater !ash to !ash of any carry-o%er caustic salt drier for drying and clay filters for impro%ing colour stability of treated product. #lay adsorbs coloured nitrogen compounds. DETAILED DESCRIPTION OF P!I DIAGRAM

'erosene0(&" as obtained from distillation unit stripper under flo! control is charged to the unit charge pumps <47 PE(0.. Pretreatment for kero0(&" consists of coalescer for remo%al of !ater and caustic pre!ash for remo%al of hydrogen
- 10 -

sulphide, etc. &he feed goes to coalescer <47-H-F !here feed passes through pass blanket as coalescing media to coalesce tiny !ater droplets into sufficiently big droplets !hich settle do!n in the !ater boot pro%ided in the coalescer. "loat type trap is pro%ided in the !ater boot to drain !ater. Aater from boot !ill ha%e to be periodically drained to oily !ater se!er. Pro%ision also e ists for bypassing this %essel and directly feeding to caustic pre!ash %essel. 'ero0(&" from coalescer is sent to caustic pre!ash %essel <47-H7 2E7C< mm /+ F7C< mm3 !here the feed bubbles through caustic and rises to the top of %essel due to gra%ity differential bet!een feed and caustic. &he feed is charged into the %essel through a distributor pipe mounted inside the %essel and holes drilled to a specified pattern on the distributor pipes. &here are three inlet no;;les pro%ided on the %essel. >ormally the feed should be maintained thro* the .I no;;le. )aintain caustic le%el and charge caustic !hen the caustic is spent as indicated by its strength. &he %essel is also pro%ided !ith a !iremesh in its top portion to remo%e any caustic entrainment. &he feed is then mi ed !ith air as necessary for reaction, on flo! control <47 "5# 76 in the air-mi er <47 K4 !here intimate mi ing of air and feed is achie%ed. &he feed then passes on to t!o reactors operating in parallel 2<47 5: (B.3 2E<<< mm /+ 74<< m3. &he reactor consists of a bed of charcoal impregnated !ith )ero catalyst. :mpregnation being carried out as per laid out procedures using ammonia as an agent for impregnation. &he reactor bed also may need !ater !ashing and reimpregnation to restore acti%ity !hene%er catalyst acti%ity drops. the period depending on the type of feed proceesed in the unit. &he feed e reactors is passed on to the caustic settler <47 H4 2D6<< mm /+ 744<< mm3. :n the caustic settler. re-uired settling time is pro%ided for separation of any carry-o%er caustic. Since the unit is also designed to treat (&", !hich has to meet stringent specifications, !ater !ash and salt drier also ha%e been pro%ided. $ydrocarbon from caustic settler passes into !ater !ash %essel <47 HD 2E7C< mm /+ F7C< mm3. &he !ater !ash %essel is continuously charged !ith demineralised !ater taken from the refinery source through a !ater tank <47 H7 pro%ided !ith a le%el controller <47 L# 47 !hich regulates !ater entry into !ater tank. "rom the !ater tank, !ater is charged into !ater !ash %essel by pump <47 PD ( B .. "lo! control is by <47 ":# 4E. Aater hydrocarbon interface le%el is maintained by <47 L# 4E. &he %essel is also pro%ided !ith a !ire mesh in its top section to reduce !ater carry-o%er by hydrocarbons. (fter !ater !ash, hydrocarbon stream enters the salt drier <47 HE 2C<<< mm /+ 8<<< mm3 for remo%al of any last traces of !ater. &he salt drier is filled !ith rock salt and the feed is distributed at the bottom of the %essel and lea%es from the top. &he final step of treatment is filtering through clay to!ers to remo%e !ater insoluble contaminants. "or this purpose t!o clay filters <47-HC (B. 2E7C< mm /+ 7C<<3 ha%e been pro%ided !hich are operated in parallel. &he hydrocarbon is distributed on top of clay filter and collected from the bottom using collector pipe assembly !rapped !ith !iremesh screens. &he outlet of each clay filter is combined into a common product run do!n line !here flo! is recorded by <47"5J:-CC. &he necessary back pressure to the unit is maintained by <47-P:#-D4
- 11 -

!hich ensures constant pressure in the reactor and other %essels. &he treated product is run-do!n to storage. "eed stocks !hich do not call for complete treatment but !hich meet product specifications after caustic pre-!ash, can be di%erted to storage after caustic pre!ash, %essel <47-H7 using the bypass line bet!een <47-H7 outlet and upstream of <47-P:#-D4. "or meeting the re-uirement of caustic for all )ero units, t!o caustic storage tanks <47- &7 B <47- &4 ha%e been pro%ided in this unit. <47- &7 is meant for preparing and storing D deg. .e caustic re-uired for caustic , pre!ash %essel <47H7. <47- &4 is meant for 7< deg. .e caustic re-uired for reactors and other )ero units. &his unit recei%es E8.8 deg .e caustic from !hich D deg. .e and 7< deg. .e caustic solution !ill be : prepared. +) !ater is used for diluting caustic. &he air re-irement of all )ero units is met by air compressors <47-#7-( B .. #ompressed air from <47-#7-(B. is supplied to other )ero units. I. PRE-COMMISSIONING OPERATIONS' C#EC ING OF COMPLETION OF CONSTRUCTION INSPECTION AND "OXING UP OF EQUIPMENT WOR (

(ll unit e-uipment and pipelines must be checked to see that they conform Strictly to the specification of design and as per dra!ings. Location of %ents, drains, gauge glasses, pressure gauges, sample points etc. on e-uipment must be checked to ensure that they are installed in accessible locations. (lso, the internal fittings in columns and %essels like trays, packing supports scre!s, distributors etc. must be checked in position and in order. Ahen the e-uipments ha%e been satisfactorily cleared as to their internal installations and cleanliness of construction debris, the manholes can be bo ed up. II. PRESSURE TESTING OF EQUIPMENT AND PIPELINES '

(fter inspection and bo -up of e-uipment as mentioned abo%e the entire unit has to be pressure tested !ith !ater to ma imum allo!able pressure to ensure that the plant e-uipment and lines can safely !ith-stand operating pressures. (ccording to con%enience, e-uipment are tested indi%idually or di%ided into sections depending on locations and test pressure of %arious e-uipment and pipelines. proper isolation by blinds of e-uipment or section under test must be done so as not to o%er pressurise connected lines and %essels of lo!er pressure rating. .efore the hydrostatic test is undertaken, relief %al%es and orifice plates must be remo%ed from the system and blinded off. (fter carrying out hydrostatic tests on unit e-uipment and pipelines !ater must be drained out completely. :n order to pre%ent %acuum pulling in %essels, their top %ents must be opened up before attempting to drain !ater. III. WATER FLUS#ING OF T#E UNIT '
- 12 -

/n completion of pressure test of the unit, !ater flushing of the different systems in the unit is carried out !ith all the pumps running on line to flush out all muck, scale and other construction debris contained in the lines. Suction screens must be installed on each pump to protect them from damage. :n the initial stages of commissioning of the unit, it is better to install a finer 26<I3 mesh on the normal filter of each pump. &his finer filter can be remo%ed only 4 to D months of actual run of the unit !hen fre-uency of cleaning comes do!n to normal. &he pumps are to be run at least for 4E hours to ensure that they are running freely and smoothly. &he discharge %al%es of the pumps ha%e to be suitably throttled so as not to o%erload the motors during the !ater flushing operations. Periodically, the pumps ha%e to be stopped and the debris accumulated in the suction screens to be cleared. &his operation has to continue till the suction screens remain clear continuously at least for eight hours. Ahen the !ater flushing operation has been successfully completed, all !ater from the systems has to be drained out completely, especially from the lo! points. (ir blo! the system thoroughly to remo%e the traces of !ater from e-uipment and lines. (ll orifice plates should be checked for proper specifications before their installation in place. (ll instruments must be checked and calibrated before the unit start-up. I$. SCREENING AND LOADING OF ACTI$ATED C#ARCOAL SALT ! CLAY

(cti%ated charcoal has to be screened properly before it is loaded in the reactors. Screening is done !ith 7< to D< mesh sie%e screens. &o re@ect fines etc. !hich are formed during transportation and handling coarser than 7< mesh and fines after D< mesh are re@ected from the charcoal supply. &he reactors are isolated from other e-uipment and their top and side man !ays are opened up. &he inlet distributor pipe assembly at top has to be suitably co%ered to pre%ent any charcoal entry into the distributor !hile loading. Loading is done through a hopper and ad@ustable loading sock !hich e tends to the bottom of the reactors. (s the loading progresses, the length of the sock is ad@usted so that no cone formation occurs on the charcoal surface. :mproper le%eling !ill cause maldistribution of hydrocarbon flo! through the bed. Loading personnel must !ear dust masks co%ering the nose and the mouth to pre%ent inhalation of charcoal dust. Ahile loading, it must be ensured that the bottom Lohnson screen collector pipe assembly is fully submerged in charcoal by physical checking from the bottom man !ay. &he person going inside for checking must !ear a fresh air masks. &he bottom man !ay is then bo ed up and loading continued !ith the sock till the inlet distributor pipe is 4D< mm from the charcoal bed. &he &op surface of the bed is le%eled after the dust has settled. $ere again, the person entering the reactor for le%eling the bed must !ear a fresh air mask. ( record of loading in the reactors has to be kept for reference and accounting, Ahen loading to the re-uired height is o%er, the loading hopper and sock are remo%ed the inlet distributor co%ering is taken off and the top man !ay bo ed up properly. $. ROC SALT LOADING '
- 13 -

(fter inspection of salt drier internals for cleanliness and fittings, it is loaded !ith rock salt up to a height of 6<< mm belo! the top tangential line. &hen the top man !ay is bo ed up. &he surface must be le%eled similar to the procedure follo!ed for charcoal loading. $I. LOADING OF CLAY IN CLAY FILTERS'

&he clay filters are checked for internal fittings and are cleaned up dry, prior to loading clay. &he inlet distributor pipe has to be co%ered suitably to pre%ent clay entering into it !hile loading. &he recommended grade of clay of the correct mesh, D<-6<, is loaded from the top of the %essels. periodically le%eling the surface so that no cone formation takes place. &he loading personnel going inside the %essels for le%eling must !ear dust mask. &he height of loading in each reactor !ill be up to F4< mm from the top tangential line. (fter le%eling of the top surface of clay in the filters, their distributors are unco%ered and the top man !ays can be bo ed up. $II. IMPREGNATION OF C#ARCOAL "ED REACTORS WIT# UOP REAGENT F". IN ERO/ATF MEROX

&he t!o reactors !ill be impregnated as a rule one after the other, as noted belo!, Start filling 47 5 7 ( !ith +) Aater. .lock off 5eactor outlet lines. Start circulation pump 47P-4 after +) !ater le%el is 7 metre belo! top distributor pipe. #ontinue to fill +) !ater. Ahen !ater le%el rises to 7 metre abo%e the distributor pipe, stop addition of +) !ater 2 .e careful, not to float charcoal out of reactor 3 #ontinue !ater circulation for 4 to D hours Start (mmonia gas in@ection after the cylinder is connected in to the circulating !ater. 5egulate the outlet pressure at D.< kg0cm4, in@ect appro imately 7C< kg of (mmonia in about C to 6 hours time. 29ach cylinder lasts for 4 704 hrs3. )easure the rate by keeping the cylinder on a !eigh bridge. 'eep a steam hose playing at the gas in@ection pipe to pre%ent free;ing on the line. #irculate the (mmonia solution for about 4 to D hrs. keeping the pump capacity to ma imum i. e. C8 )D0hr . Sample the solution and send to lab for analysis. (mmonia concentration should be <.4 6 or - <.<4 !t. G. (dd or dilute the solution as necessary. )ean!hile get the catalyst dissol%ing drum system ready !ith the hoses connected. /rdinary drum of 4<< liters !ill sol%e the purpose. (fter achie%ing the re-uired (mmonia concentration in the circulating !ater. route a slip stream from 47 P4 discharge to the catalyst drum. "ill it up to C< to 6<G. Start gentle air blo!ing in the (ir Sprayer.

- 14 -

(dd 7 bottles of )ero ". after shaking. Stir the mi ture to help dispersing the catalyst if re-uired. )ake up the %olume to 78< litres. Start educting the catalyst solution by routing the slip stream through the eductor 47 G-4 from 47 P-4 discharge to suction. 5egulate the catalyst eduction rate to D to E litres0minute. (fter establishing the abo%e rate, fill the drum from Pump discharge !ith a rate e-ual to eduction rate. (dd 7 bottle of )ero ". e%ery 7< minutes. (fter about 7704 hrs. start checking the color of the circulating (mmonia at the pump suction before educting point. &his color should be clear or faint blue. :f the color is dark blue, it means that there is channeling in the charcoal bed :n such a case the impregnation is to be stopped and 5eactor bed should be flushed !ith air to rectify the bed channeling. (dd EC bottles of )ero ".. (fter the last batch of solution is educted, flush the catalyst drum se%eral times !ith (mmonia solution and educt to the 5eactor . #ontinue circulation for about E hrs. Start transferring (mmonia solution to the second reactor 57 . by opening the inlet block %al%e to top distributor !hen the solution le%el in 57 ( falls belo! top distributor, shut off the inlet and continue to transfer all the circulating (mmonia solution into 57.. Ahen the pump loses suction shut off the pump. .lock in 57(. /pen hydrocarbon outlet from 57 . and start circulation back to the inlet. Start taking +) !ater to fill 57 . until the le%el is 7 metre abo%e the distributor pipe. Stop +) !ater flo! to the 5eactor, but continue the circulation. Sample the solution and analy;e for (mmonia concentration. :n@ect (mmonia gas again into the circulating solution to get <.4 6 or - <.<4 !t G. :mpregnate 57 . charcoal bed similar to 57 (. 2(dd EC bottles of )ero ".3. (fter completing the impregnation of both charcoal beds, the circulating solution can be discarded to se!er. +rain out all the remnant (mmonia solution from both reactors to se!er. "lush and drain each reactor !ith +) !ater to remo%e residual (mmonia 2keeping checking the effluent p$3. #lose the top man !ays of both reactors. Start alkalising each reactor bed !ith 7<G caustic soda solution and then circulate the same for 4 hrs. (bout 8)D of >a/$ for each reactor !ill be sufficient.
- 15 -

>o! the reactors are ready for commissioning !ith 'ero0(&". 5e-uirement of #atalysts0#hemicals, 2a3 2b3 2c3 $III. )ero ". catalyst (mmonia +) !ater -F< .ottles. -C #ylinders of 6< 'g net !t. -4C< )D

C#ARGING OF C#EMICALS'

&he caustic storage tanks <47- &7 and &4 are meant to prepare and store D=.e and 7<=.e caustic solutions respecti%ely in them. &hese t!o tanks take care of the caustic re-uirements of all the fi%e )ero units. 46.C=.e* caustic is recei%ed in the unit tanks prior to unit start-up. &he caustic is then diluted and the solution of re-uired strength prepared in each tank. D=.e* caustic is used for pre-!ash in %essel <47-H7 !hile 7<=.e. #austic is used in the reactors 57( and . as !ell as in other )ero 1nits. Solutions of re-uired strength are prepared in the unit by diluting !ith demineralised !ater. START UP PROCEDURE

(s soon as 'erosene0(&" becomes a%ailable from the (tmospheric Hacuum +istillation 1nit, slo!ly fill up the unit %essels %i;., the coalescer HF, caustic pre!ash %essel H7, )ero 5eactors 57( and 57 .. caustic settler H4, !ater !ash %essel HD, Salt +rier HE and the clay filters HC( and HC. one by one. 9nsure all air from the resepcti%e %essels is remo%ed by opening the top %ents. before filling them !ith the product kerosene0(&". Proceed further, as follo!s, "ill up D=.e* caustic solution in the pre-!ash column H-7 to the specified operating le%el so that the kerosene0(&" stream bubbles through caustic solution !hich !ill absorb all the hydrogen sulphide and naphthenic acid contaminants from the feed stock. :n a freshly charged )ero reactor no circulation of caustic is needed in the beginning. $ence commissioning the feed charge pumps <47-PE (0. 'erosene is charged through the coalescer. pre-!ash column, reactors and caustic settler and the pressure are raised in the %essels to their normal operating le%els. Setting the back pressure controller <47-P#-D4 on the product rundo!n line, for gi%ing the desired pressures in the %essels, air in@ection to the mi er <47-K-4 is started at the specifed rate through flo! controller "5#-76. &he rate of air is appro imately D< lbs0lb of mercaptan sulphur in the feed. &he back pressure controller P#-D4 is set such that all air used for the process is kept in the hydrocarbon solution. :nitially, the product after treatment is to be routed to the slop tank. Ahen doctor test is consecuti%ely negati%e for 4 hours the kerosene stream may be routed to its normal storage tanks.
- 16 -

Aater !ashing the product to remo%e the entrained caustic has to be done. $ence, start !ater-!ashing the product, pumping +) !ater into the !ater !ash %essel <47-HD on flo! control "7#-DE through the distributor in the %essel. ( steady le%el has to be maintained by operating the controller L#-4E !hich controls the spent !ater effluent from H-D bottom. &he !ater !ashed product stream is passed through the drier !hich remo%es traces of !ater carried o%er. "inally, route the product through the clay filters <47HC( and . to remo%e !ater insoluble contaminants and gi%e clarity to the product. (fter passing the -uality control tests !hich are %ery stringent in the case of (&", the product is routed to the normal storage tanks. /ff-spec material !hen treating (&" stream is di%erted to 'erosene tanks. :f the feed 'erosene contains %ery little mercaptans i. e. less then 7< ppm, then the entire )ero treatment may not be re-uired at all. :t can be directly routed to run-do!n by-passing the treating section. :n cases !here feed contains traces of $4S. but %ery less mercaptans, the feed can be routed through caustic pre-!ash and then direct to product run-do!n by passing reactors etc. Ahen the plant has been fully in operation, set the feed rate to the desired le%el. #heck the air in@ection rate for mi ing before reactors is ade-uate and ensure proper le%els are maintained in all %essels. Pressure, as already mentioned has to be set by the pressure controller P#-D4 on the product rundo!n line. I. REACTOR "ED WATER WAS#ING ! REIMPREGNATION WATER WAS#ING

/%er a period of time, the catalyst impregnated on charcoal in the reactors loses its acti%ity. Aetting the catalyst !ith fresh caustic circulation also may not help in bringing the product to specifications. (t this stage, the charcoal bed has to be hot !ater !ashed to remo%e the organic and soap deposits from its pores and bring back the acti%e surface of the catalyst, for reaction. &his deposition of cold organic material on charcoal takes place gradually and hence the !ater !ashing step can be con%eniently planned to suit the product re-uirements. &he !ater used for this !ashing must be free of dirt, suspended matter, hardness salts and acti%e chlorine. $ence, steam condensate or +) !ater is used for !ashing. Proceed as follo!s, Stop air in@ection and hydrocarbon charge to the reactors. Pump out all the kerosene0(&" from the bottom of the reactors under steam pressure. Steam out the reactors for about an hour gi%ing steam through the beds at a rate e-ual to 7< lbs per cu feet of bed, i. e. about 7E )&0hr for each reactor. #ommission the !ater heater <47-L7 and start gi%ing hot !ater at a temp. of about 8C-FC=# to the reactors through the distributor pipes at a rate of 8 gallons0minute for 7<< cu. feet of charcoal i.e. about CC ) D0hr. fill up the reactors and then drain them to the se!er at the same rate as filling !ater into them.
- 17 -

:t !as e perienced that !hile using !ater heater 247 L73 lot of hammering !as taking place resulting se%ere %ibration of the lines and therefore it !as difficult to maintain the !ater temp, Later on ."A line connection !as gi%en d0s of +) Aater .0H. &his does not re-uire !ater heater ser%ices. ."A temp. can be controlled by controlling the steam to deareator. :nitially, the draining effluent !ill be dark bro!n and foamy !hich !ill change colour and e%entually becomes colourless. Ahen the !ater from the drain is clear and clean, the !ater !ashing can be stopped. Stop the !ater flo! and blo!out as much !ater as possible from the reactor beds !ith steam gi%en to reactor top. 'eep the steam flo! through the beds for another D< minutes to remo%e as much residual hea%y oil as possible from the charcoal bed. Stop steam in@ection and block off !ater heater. :ntroduce air into the reactors and blo! the reactors !ell for an hour or so that there is no !ater drip noticed from the bottom drain. >e t alkali;e the beds !ith fresh 7< deg. .e caustic solution and then return the unit to normal !orking condition as discussed under IStart-up ProcedureI. II. CATALYST REIMPREGNATION

&his step is necessary only !hen hot !ater !ashing, higher feed temperatures, stronger caustic saturation, reduced feed rates etc., do not help in mercaptan o idation and the product remains doctor positi%e. &he reimpregnation inter%al may %ary from three months to one year depending on proper pre!ashing feed mercaptan content, crude source etc. III. REIMPREGNATION OF EROSENE/ATF REACTORS

$ot !ater !ashing. (cidising the reactor bed. :mpregnation I$. #OT WATER WAS#ING

:solate 5eactor 247 5-7 (3 from the rest of the unit. Start pumping out the kerosene, keep reactor under positi%e pressure by steam. (fter kerosene is pumped out, start steam flo! from the !ater heater 247L-73 to the 5eactor 2'eep the bed temp. 7F< deg #. +rain out the condensate from 5eactor bottom. &his is to remo%e the residual kerosene and hea%y hydrocarbon in the bed. Start introducing +) Aater through the !ater heater into 5eactor. 'eep the !ater temp. 247 &7-7C3 around F<-FC deg # by introducing steam into the !ater heater.
- 18 -

Ahen the 5eactor is full, open reactor bottom to drain. 'eep the drain rate close to the hot !ater fill rate i.e. about C< )D0hr. >/&9, :nstead of using !ater heater, ."A can directly be taken.

#heck the drain !ater color. Ahen the colour is clear, check the reactor effluent p$. #ontinue hot !ater !ashing till reactor effluent p$ is do!n to 8,F. "ollo! step 7.7 to 7.C for another reactor 2475-7.3 and 4D5-7. $. ACIDISING OF REACTOR "ED'

Stop the !ater and steam flo!. "lush out the caustic circulation system by opening up the suction lines from the reactor bottom to the circulation pump 47 P-4 and pump discharge to spent caustic tank. /pen the top man!ay of the 5eactor. 5efill reactor 247 5-7(3 !ith +) !ater after the reactor has been pumped out till !ater le%el is 7 ) belo! the distribution pipe, .lock in 5eactor outlet line. Start circulation from bottom to top of the reactor. .oth the kerosene outlet and the bottom pump out of the reactor are open to the pump suction. #ontinue to fill +) Aater till !ater le%el is 7 ) abo%e the distributor pipe. :n@ect steam occasionally to keep the circulating !ater temp. at C<-6C=#. &ake about <.7 )D glacial acetic acid to the (cetic acid addition pot 47H-8. 5oute a slip stream from the circulating pump discharge to the eductor 47L-4. Start educting acetic acid to the circulating system B it should be added to the system o%er a C-7< minutes period. (fter circulating acidified !ater for about one hour check the reactor effluent p$. :f p$ is higher than 6.C, add another batch of about <.7 ) D, &his acetic acid addition is necessary to neutralise the trace alkalinity on the bed and to pro%ide a slight acidic medium. &ransfer the acidified !ater to reactor 47 5-7. and continue the circulation in 47 5-7(, Stop circulation !hen the le%el is 7 ) belo! the distributor pipe. "ollo! step 4.6 to 4.8 for acidising the bed of 475-7.. &ransfer the acidic solution to 4D5-7 from 47 5-7. !ith circulation on. Stop circulation !hen le%el is 7 ) belo! the distributor pipe. 'eep a moderate steam flo! through each reactor for D<-6< minutes. (ir purge each reactor for about 6<-F< minutes.
- 19 -

$I.

IMPREGNATION

Start filling reactor 47 5-7( !ith +) !ater. .lock in reactor outlet lines. Start circulation pump 47 P-4 after reactor le%el is 7 ) belo! the distributor pipe, #ontinue to fill +) !ater. Ahen !ater le%el rises to 7 ) abo%e the distributor. Stop !ater addition 2.e careful not to flood the charcoal out of the reactor3. #ontinue circulation for about 4-D hours. Start (mmonia in@ection after the cylinder is connected. 5egulate the outlet pressure at about D kg0cm 4. :n@ect appro . 7C< kg of ammonia i.e about C-6 hours 2one cylinder in 4-4704 hrs.3 )easure the rate by !eighing scale. Put steam hose to pre%ent free;ing of pipe due to gas e pansion. #irculate ammonia for about 4-D hours keeping the rate at pump ma imum i. e. C8 )D0hr. Sample the solution and send to lab analysis. (mmonia concentration should be <.4 6 or - < <4 !t.G. (dd or dilute solution if necessary. (fter confirmation of solution concentration, route a slip stream from 47 P-4 discharge to the catalyst drum 24<< litre drum3. "ill it up to C<-6<G. Start gentle air blo!ing in the air sprayer. (dd 7 bottles of )ero ". after shaking. Stir the mi ture to help dispersing the catalyst, if re-uired. )ake up the %olume to 78< litres. Start educting the catalyst by routing the slip stream through the eductor 47L-4 from 47 P-4 discharge to suction. 5egulate the catalyst solution rate at about D-E litre0min. (fter establishing the eduction rate, fill the drum from pump discharge !ith a rate e-ual to the educting rate. (dd 7 bottle of )ero ". e%ery 7< minutes. (ppro . after 7704 hour start checking the colour at pump suction before the educting point. &he colour of the solution should be clear as a %ery light tint blue. :f the blue colour is obser%ed, impregnation must be stopped B reactor bed be *fluffed* !ith air to correct bed channeling. (dd EC bottles of )ero ".. (fter the last batch of solution is educted, flush the catalyst drum se%eral times !ith ammonia solution and educt it into the reactor. #ontinue circulation for about E hours.

- 20 -

Start transfer ammonical solution to reactor 47 5-7 . by opening the inlet distributor block %al%e. Ahen the le%el in reactor 475-7( falls belo! the distributor pipe, shut off the inlet. #ontinue0transfer to ammonical solution into reactor 47 5-7 .. Ahen the pump loses suction, shut off the pump. .lock in reactor 47 5-7(. /pen $# outlet from reactor 475-7. and start circulation to its inlet. Start taking +) !ater to fill the reactor until the le%el is 7 ) abo%e distributor pipe. Stop +) !ater flo! to the reactor but continue circulation. Sample the solution and analyse for ammonia. :n@ect ammonia to get <.4 6 or - <.<4 !t. G of ammonia in the solution. :mpregnate 57 . charcoal bed in the same as !ay as that of 57 ( 2add EC bottles of )ero ".3. (fter impregnation, ammonia solution is to be transferred to H. >aphtha reactor 2&o be impregnated3. +rain out all remaining ammonia solution in both reactors. "lush and drain each reactor !ith +) !ater to remo%e residual ammonia, 4 hours is ade-uate. Sample the charcoal in plastic bag for each reactor at three0four points. #lose the top man!ays. Start alkali;ing each reactor !ith 7C=.e* caustic, use 8.C ) D of caustic for each reactor. #irculate the solution for 4 hours. &he reactors are ready for kero0(&" introduction. 59J1:59)9>& /" #(&(LKS&0#$9):#(LS )ero ". catalyst (mmonia cylinder Glacial acetic acid +) Aater S#UT DOWN PROCEDURE' F< bottles C cylinders of 6< kg each

4<< litres 2appro .3 4C< )D

"or planned shut do!n for inpsection of e-uipment and maintenance !ork in the unit, follo! the steps gi%en belo!, Shutdo!n air in@ection to the mi er and shut off feed charge pumps PE(0E. to the coalescer <47-HF. Shut off !ater !ash pumps PD(0D.. 9mpty out the salt-drier and clay filters into the kerosene storage tanks.
- 21 -

:f the caustic is spent in settler <47- H4, it can be pumped out to spent caustic system for disposal. 9mpty out the reactors also of the spent caustic. 'erosene remaining in the coalescer has to be drained out. Ahen all the %essels ha%e been emptied out of their contents, they are to be isolated by blinds. .lind list of the unit has to be kept upto date. Steam and !ater !ash indi%idual e-uipment and systems to make them free of hydrocarbons, caustic etc. and safe for entry. +etailed instruction for this step !ill be gi%en at the time of actual shutdo!n. 9ntry to the %essels should be gi%en only after making sure that they ha%e been isolated properly, %entilated enough, gas tested free and safe to enter. 5ecommended safety e-uipments must be !orn by !orkman entering the %essels !hich contained caustic etc. +ust masks and fresh air e-uipment must be used !hen charcoal loading0unloading and le%elling are done inside the reactors.

EMERGENCIES'

9mergencies can result from e-uipment failure and from interruption of feed and utilities. /perators should be thoroughly familiar !ith the emergency procedures and understand the reason for each mo%e. >ature and degree of emergency %aries from time to time and hence good @udgement and discretion should be e ercised to tackle such situations. I. ELECTRIC POWER FAILURE'

:f it is a general po!er failure, feed to the unit !ill be interrupted !ith the failure of the pumps. $ence a shutdo!n of the unit is ine%itable. Shut off air in@ection to the mi er immediately and block off feed to the unit. Shut off discharge %al%e of unit pumps and close pressure controller at unit limits and hold system pressure. Start up the unit as per procedure !hen po!er supply is resumed. II. STEAM FAILURE'

Local steam failure !ill not affect the unit running immediately, but if (H1 running is affected by the emergency, feed to the unit might be interrupted. :n such a case, the unit !ill ha%e to be shutdo!n and kept in a standby condition pending resumption of feed supply from (H1. III. INSTRUMENT AIR FAILURE'

:nstrument air failure !ill result in all unit control %al%es operating in the fail-safe position, i. e., they !ill all close. #lose off feed to the caustic pre-!ash %essel H-7. Shutdo!n caustic circulation pump P7, circulation pump P4 and !ater in@ection
- 22 -

pump PD and block le%el controllers !ith isolation %al%es. )onitor all le%els. $old system pressure by blocking off pressure controller at unit limits. 5e%ert back to normal operations, starting the unit follo!ing standard procedure, once air supply to the instruments has been resumed. I$. COOLING WATER FAILURE '

( total failure !ill effect feed supply to the unit and pumps. $ence, unit !ill ha%e to be shutdo!n immediately. :solate all the pumps after stopping them. #lose the pressure controller and hold system pressure. )aintain le%els in the %essels. Startup the unit in the normal !ay, !hen cooling !ater supply becomes a%ailable and feed from (H1 is restored to the unit. $. AIR COMPRESSOR FAILURE'

:f the duration of the failure is only short, the product may not go off specification. .ut the mercaptan con%ersion efficiency drops off rapidly and the product !ill ha%e to be slopped as soon as it goes off -uality. (ir in@ection block %al%e has to be immediately shut-off to the reactors 57( and ., on air compressor failure. /n resumption of air supply, check the product -uality and !hen it is on specification, route it to storage tank. :f both the compressors are not a%ailable for a longer duration due to break-do!ns and maintenance, the 1nit !ill ha%e to be shut-do!n. OPERATING $ARIA"LES'

&he caustic solution used for )ero treatment %i;. :n pre-!ash column and in reactors become spent e%entually. Aeak acids like #/4 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 e tract mercaptans !ill suffer. $ence, it becomes necessary to remo%e part of the spent caustic and replace from time, to time to restore its alkalinity. &he feed stock should be freed of all hydrogen sulphide by passing it through the pre-!ash column. /ther!ise the o idation reaction !ill be suppressed in the reactors. :t !ill gi%e rise to increased caustic consumption. Lo!ering hydrocarbon feed rate and caustic temperature !ill impro%e mercaptan e traction >aphthenic acid in feed stock may gi%e rise to emulsion problems and hence must be remo%ed by pre!ash !ith D=.e caustic solution. / idation rate is increased by increasing the temperature and catalyst concentration. (bout D< cubic feet of free air is re-uired for each pound of mercaptan sulphur to be o idised. &he amount of )ero #atalyst needed !ill be appro imately one pound for 7<<< gallons of 4C=.e caustic solution.

- 23 -

Sufficient back pressure must be maintained at each e traction stage to pre%ent %aporisation and caustic entrainment. Presence of acid oils upto a limit of 8G !ill increase solubility of mercaptans in the caustic.

- 24 -

 Sr

C#EMICALS ! CATALYST Hessel >o. #austic4 7H7 #austic4 757(0. :nitial fill,)D F.D (ppro . le%el of initial fill D<-C<G of upper LG 5efer 7<o.e caustic tank calibrati on chart #austic strength G!t 4.7 )ake up 0 change out !hen Juantity re-uired Ahen caustic strength to 7.<G 9 pected duration !ith design crude

C7.C

6.F

(bout 7<G of 9%ery F days initial fill 2drain up to bottom LG B make up3 #irculate reactor caustic once a C7.C )D /nce in C days days. (fter about C circ. #harge caustic. #austic strength !ould be around 6.4G (bout 4C< litres reimpregnation for each (bout once months. (bout once in E months at design throughput in E

(citic acid 4757(0. (cti%ated 777 charcoal 4757(0. 5ock salt 767 24<<)&3 47HE "ilter clay 47HC(0. 1/P #atalyst ". 4757(0. 4C6

(fter e%ery D months run of the unit. #heck the salt le%el and make up accordingly F< bottles re-uired during each impregnation

F< bottles of 7.C litres each. 2acti%e ingredient per litre is <.D4C kg3
- 25 -

 I.

MODIFICATIONS ' ANTISTATIC DOSING FACILITY

&his facility is gi%en to maintain (&" conducti%ity bet!een C< to EC< psm 2P:#/ simen per meter3 to meet the specification. (ntistatic (gent is stored in a small %essel 2<.<88 )D3. &!o dosing pumps, 47P6(0. ha%e been pro%ided to dose (S( to +0S of 47P:#-D4 as per specification. II. ATF REPROCESSING FACILITY

Aith (H1 re%amp, (&" production has gone high. +uring (&" crude processing part of untreated (&" is sent to separate tank E<E directly from (H1 .0L. this untreated (&" stored in tank can be reprocessed in kero0(&" unit at the time !hen (H1 is on .$ crude processing. ( line is layed from tank E<E to unit 47. ( pump 47P7 is gi%en !hich takes suction from tank E<E. Pump discharge line @oins to 47PE(0. suction line !ith a #0H and flo! transmitter namely 247"5#E<3. &his facility can also be used for blending .$ (&" !ith imported (&".

- 26 -

%. U-22 STRAIG#T RUN LPG MEROX

UNIT CAPACITY'

&he )ero 9 traction 1nit for straight run LPG has been designed to process 7<,<<< )&0year of an essentially #D0#E mi ture obtained from the stabili;er column of the (tmospheric distillation unit. &he unit shall operate for DEC stream days in a year. FEED SPECIFICATIONS'

&he straight-run LPG feed to the )ero unit shall ha%e substantially the follo!ing properties, Hapour pressure at 6C=# # C*s mol.G Specific gra%ity at 7C.6=# )ercaptan sulphur !t. ppm. $ydrogen sulphide !t. ppm PRODUCT SPECIFICATIONS ' , 77 kg0cm4 ma . , 7.< ma . , <.C6 , F<< ma . , 4<< ma .

&he straight run LPG after )ero treatment shall meet the follo!ing specifications e cepting its %apour pressure shall not e ceed 77.< kg0cm 4 at 6C=#. &otal Sulphur !ppm, 7C ma 5S$ !ppm , C ma $4S !ppm , >il #u #orrosion , >o !orse than $4S "ree feed PROCESS DESCRIPTION'

(mine absorber for remo%al of $4S and caustic pre!ash %essel are pro%ided for pretreatment. &reatment for S5 LPG consists of only an e tractor !ith caustic, as all mercaptans present in feed are in the e tractable range. 9 traction caustic is o idised in a common o idiser section. #austic settler has been pro%ided for settling and separation of carry-o%er caustic from e tractor.
- 27 -

DETAILED DESCRIPTION OF P!ID

LPG obtained from crude unit stabiliser o%erhead is charged to unit by unit charge pumps <44P-7(0.. &he feed is sent to the bottom of amine absorber <44#7 27<<< mm 7FC<< mm3. &he column is pro%ided !ith E sie%e type trays. 5egenerated +9( from amine regenerator is recei%ed in a surge drum pumps pro%ided in cracked LPG mero unit. +9( from surge drum is pumped to the column top on flo! control <44 "5#C. 5ich +9( from column bottom is sent to amine regenerator located in .itumen0Sulphur unit area %ia le%el control <44 L# E, under column pressure. &he $4S free LPG lea%es from top of <44 #7 to caustic pre!ash %essel <44H7 2 77<< /+ 67<< mm 3 on flo! control <44 "5#J:-7. Pro%ision for bypassing 44#-7 in running condition is made by gi%ing a @ump o%er from inlet to outlet bypassing the (mine absorber. :n order to keep up the e traction efficiency constant at lo!er throughputs, a recirculation stream back to crude unit stabiliser is pro%ided. &his recirculation flo! can be maintained by flo! controller <44 95# 7D. :n LPG caustic pre!ash %essel, LPG is introduced at the bottom of the %essel through a distributor pipe. "or this purpose, three no;;les at different le%els ha%e been pro%ided. &he %essel is pro%ided !ith a !ire mesh at top to remo%e caustic mist. #austic in the %essel has to be replaced !hen it becomes spent. LPG is then sent to the e tractor <44-#-4 27<<< /+ mm 76E<< mm3 !here mercaptans are e tracted by caustic from caustic regenerator section. &he e tractor is pro%ided !ith 77 sie%e type trays. #austic is charged on flo! control <44 "5#-F. 5ich caustic from e tractor is sent to caustic regenerator section on le%el control <44 L:#-8. LPG after e tractor goes to #austic settler <44 H4 27<<< mm /+ E<<< mm3. (fter caustic settling LPG is run do!n to storage through a back pressure controller <44P#-74 to ensure constant back pressure in the 1nit. &o run-do!n LPG, mercaptan is added from odorant pot <44H<D by odorant pumps <44P<4 to maintain odour specification. #austic from settler can be drained into e tractor caustic line going for regeneration. >/&9, )ercaptan dosing pumps ha%e been remo%ed for some other ser%ices and dosing lines ha%e been blinded as dosing is not re-uired.

- 28 -

 I.

PRE-COMMISSIONING OPERATIONS' C#EC ING COMPLETION OF CONSTRUCTION WOR S( INSPECTION AND "OXING UP OF EQUIPMENTS

&he follo!ing preliminary operations ha%e to be carried out to ensure a successful start-up of the unit, #heck that all mechanical !orks of construction ha%e been completed, e-uipments inspected, bo ed up and signed off on unit check lists made for this purpose. Scaffolding, debris, tools and other construction materials remo%ed from the unit area. )ake a final list of blinds !hich should be in position or taken out before starting purging operations. )ake sure all blinds ha%e been installed at the proper sides of %al%es and signed off in the list. #heck and ensure "ire-fighting and safety e-uipment is in place and in good !orking condition. 9nsure all utility systems and flare release headers are in ser%ice and ready for use. :solate the unit from other plants and tankages at the unit limits !ith block %al%es. 'eep the fuel gas and flare header isolated from the unit pending purging operations. :solate or remo%e orifice blocks of all flo! meters for flushing purposes. II. WATER FLUS#ING OF T#E UNIT '

"or !ater flushing of a ne! unit, use ordinary !ater. Aater flushing of the entire unit has to be done !ith all pumps running on line so that all muck, scale and construction debris are !ashed out of all e-uipment and unit pipelines. &he unit can be con%eniently taken in sections or indi%idual e-uipment !ise and the flushing operation is carried out !ith temporary connections from the "ire !ater header. Suction screens ha%e to be installed on the pumps during the flushing period to protect them from damage. &hey ha%e to be run at least for 4E hours continuously to ensure their free and smooth ser%ice. +uring the flushing period, care should be taken to throttle the pump discharge %al%es suitably so as not to o%erload the motors. &he screens on the pump suction lines ha%e to be cleared off all debris collected periodically after stopping the pumps. till they remain clear continuously at least for eight hours. +isconnect all instruments lead lines and flush the leads thoroughly. )ake sure that all process lines, control %al%e loops are thoroughly flushed, to atmosphere to remo%e muck, construction debris, etc. .etter to drop each #0H and flush the assembly and bypass also thoroughly. &hen the #0H can be refi ed in position. )ake sure all lo!
- 29 -

points bleeders are clear and all columns and %essels %ents and drains should be clear. Ahen !ater flushing operation is completed, !e ha%e to pressure test the entire unit !ith !ater as detailed belo!, :::. PRESSURE TEST OF EQUIPMENT ! LINES ,

:n order to check for leaks on e-uipment and lines after !ater flushing, they are all sub@ected to !ater pressure of about 76-4< kg0cm4 ."or this purpose LPG inlet to amine scrubber and its outlet after the pressure controller are isolated by block %al%es. 5ich amine and rich caustic outlets from scrubber 44#7, pre-!ash %essel 44H7, e tractor 44#4 must also be blocked off. :nitial filling of the entire unit can be done !ith "ire !ater for remo%al of air. "or pressurising !e ha%e to use .oiler feed !ater. 'eep running the pump out of 7F P7E (0.0# group and through the permanent supply line take ."A to this unit and slo!ly pressurise the entire system to normal operating pressure for a period of 7C to D< minutes. :f necessary one or t!o drains may be kept open to ha%e a small discharge from the pump. +uring pressure test safety %al%e do!n-stream flanges may be kept !edge open or to check tight shut-off of safety %al%es before their set pressure. &ighten all leaky flanges, %al%es glands etc. !here re-uired. Gaskets may ha%e to be replaced after pressure test. 'eep a record of such flange @oints for subse-uent testing before cutting in of feed LPG. (fter the system pressure test is successfully completed depressurise the unit, but keep the system filled !ith !ater. >o! the system is ready for taking in "uel gas. &his is the best !ay of keeping air out of the unit. LPG can be taken in to the unit from (tmospheric 1nit in small -uantities. LPG can be lined up slo!ly to pressurise the unit to a slight positi%e pressure !ith gas. &his has to be done slo!ly and carefully to a%oid chilling. :f. ho!e%er, fuel gas is a%ailable, gas can be taken directly. LPG %apourises slo!ly gi%ing positi%e pressure. >o! drains off the !ater from the entire system under gas pressure. :H. C#ARGING OF C#EMICALS ,

(fter pressurising the unit !ith fuel gas, inlet %al%e to the scrubber 44#7 is blocked off. 9nsure that +9( inlet and outlet from 44#7 are also blocked off. Similarly, ensure that caustic charge line to 44 H7 and its e it as !ell as )ero coustic inlet to e tractor 44 #4 are all shut off. &he )ero regeneration system is also pressured up !ith fuel gas upto the disulphide separator in cracked LPG )ero unit and the e tractor 44#4 bottom %al%e is blocked off. )ake sure air inlet %al%e to the o idiser <4E-HD remains blocked off. (lternati%ely regeneration section can be filled !ith caustic and %ented at suitable points to remo%e air . :n preparation for charging chemicals into the unit, %ent gas from the caustic regeneration system till the system pressure drops to <.C kg0cm 4. prepare 4<= .e
- 30 -

caustic solution in the storage tank pro%ided and transfer to disulphide separator <4E-HE,!ith a good le%el in 4EHE, start circulation pump <4E-P7(0. and establish a le%el in LPG e tractor 44#4. &hen line up the pump 4EP7 (0. for circulating caustic to e tractor 44#4, through bottom L:# to the caustic heater <4E-97, o idiser <4E-HD and back to disulphide separator <4E-HE. (d@ust the circulation on "5# control at the stipulated rate. "rom the 7<= .e caustic solution tank in 'erosene )ero unit, transfer enough material into pre!ash %essel 44H7 to hold sufficient le%el. Line up lean +9( from sulphur 5eco%ery 1nit and establish !orking le%el in amine scrubber 44#7. 9stablish +9( circulation putting into commission the le%el controller at bottom of the column to control the rich amine solution returning for regeneration in the sulphur reco%ery unit.

START-UP PROCEDURE,

(fter the precommissioning acti%ities ha%e been completed and all e-uipment and piping etc. are purged to remo%e air proceed as follo!s, 9stablish )ero caustic circulation to top of e tractor column 44#4 after establishing a !orking le%el in disulphide separator 4EHE in cracked LPG )ero 1nit. !hen normal le%el of caustic is obtained in 44#4, commission the bottom le%el controller to regulate rich caustic flo! back to disulphide separator 4EHE. #harge lean amine on flo! control to the amine scrubber 44#7. )aintain le%el at the bottom of 44#7 by commissioning the le%el controller regulating the rich amine flo! to regenerator section in (51. Lining up the product flo! upto the rundo!n %al%e at battery limits, charge straight run LPG to the amine scrubber by means of pumps P7( and .. #ontrol the flo! rate from the scrubber to the caustic pre!ash %essel 44H7 !ith the "5# on line. 5oute LPG to rundo!n passing through the e tractor 44#4 and caustic settler 44H4 displacing all the fuel gas to a horton-sphere lined up at LPG recei%ing station. Ahen operating conditions become steady, !ith the le%el controllers of 44#7 and 44#4 maintaining ade-uate le%el, ad@ust the flo! rate of LPG to the pre!ash %essel 44H7 to normal rate. #ommission the recycling line of LPG back to the stabili;er column of (H1. 1se the recycle line if 44#7 operates at lo! throughputs. /perate the rundo!n line pressure controller to maintain the desired back pressure in the system. #heck the product after caustic settler for -uality. Ahen it is doctor negati%e. it can be routed to the regular storage spheres, kept ready for the purpose.

- 31 -

#ommission odorant in@ection to the rundo!n LPG after caustic settler at the specified rate. #heck the odorant in@ection facility is ready in all respects beforehand. &hen start the in@ection pump 44P4 and set dosage. as instructed. >/&9, /dorant in@ection is no more in use no!adays.

#heck fre-uently LPG for $.S after the pre!ash %esel7 44H7 and replace caustic as necessary. 44H7 caustic is be replaced !hen caustic becomes C<G spent. #heck the regenerated caustic being charged to the e tractor 44#4. "or e tractable sulphur in it. &his !ill gi%e an idea of the efficient operation of disulphide separator.

S#UTDOWN PROCEDURE,

:nform all concerned of intention to shutdo!n the unit and proceed as follo!s, Shut off +9( charge pump to the scrubber 44#l. Shut off LPG charge pump to 44#7 immediately after this. Stop odorant in@ection pump 44P-<4. Stop caustic circulation through the e tractor 44#4 from the disulphide separator 4EHE. Stop caustic supply to pre-!ash %essel 44H7. 9mpty out caustic le%els from 44H7, 44#4 and 44H4 to spent caustic disposal or to the disulphide separator 4EHE in the cracked LPG )ero unit, as instructed. 9mpty out +9( le%el in 44#7 to its regeneration section in .itumen0Sulphur area. +epressure the %essels and columns slo!ly to the flare system, after isolation at unit limits. :solate the %essels and columns by blinds and make them gas and chemicals free by !ater !ashing repeatedly, as per special instruction that !ill be issued at the time of shutdo!n. 'eep an upto date record of the blind list. 9ntry to the %essels has to be gi%en 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 gi%en. Proper %entilation inside the %essels must be ensured. Personnel entering the %essels must !ear proper protecti%e e-uipment as mentioned in the clearance permits.

- 32 -

 :.

EMERGENCY PROCEDURE POWER FAILURE,

:n case of general po!er failure LPG supply to the unit !ill stop and the unit pumps running !ill be interrupted. +9( solution circulation also !ill stop. .lock off pressure controller at unit rundo!n line and hold pressure in the system. )onitor all le%els. Ahen po!er supply and LPG feed are restored, put the unit back into normal operation, follo!ing standard procedure. ::. STEAM FAILURE,

:n case of general steam failure, LPG to the unit !ill be affected and hence unit !ill ha%e to be shut do!n and kept under pressure till feed supply is resumed from (H1. :f the steam failure is confined to the )ero unit only then LPG )ero section can run !ithout any interruption. :::. COOLING WATER FAILURE ,

"ailure of cooling !ater !ill affect the feed supply to the unit as !ell as the unit pumps. 1nit !ill ha%e to be shutdo!n and kept standby till !ater supply is restored. :H. INSTRUMENT AIR FAILURE,

/n instrument air failure, all the control %al%es in the unit !ill close. :f (H1 is also affected by air failure, feed to the unit !ill be interrupted. #lose off the pressure controller on LPG rundo!n line and maintain pressure in the system. )onitor all le%els till air supply is resumed to normal. 5e%ert to normal operation. :. OPERATING $ARIA"LES , LPG PREWAS# ,

LPG is passed through amine scrubber 44#7 and caustic pre!ash %essel 44H7 to remo%e all traces of hydrogen sulphide. &he +9( solution should be kept at the specified %alue of 4CG by !t. &he amine circulation rate also should be at the design rate of about 8<< kg0hr. #austic concentration for pre!ash should be 7<4<= .e, !hen it becomes spent, caustic must be replaced !ith fresh stock. ::. LPG 9M&5(#&/5,

)ercaptan e tractor 44#4 remo%es these undesirable components from LPG stream by intimate mi ing !ith a caustic solution containing )ero catalyst. &he caustic concentration for the circulation should be 4<= .e. &he catalyst
- 33 -

concentration in the caustic should be 7<< ppm. )ero solution circulation rate should be <.77 )D0hr. /perating pressure !hich is maintained by the pressure controller on the rundo!n line should be about 78.< kg0cm4 at the e tractor 44#4. 5educing any of these %ariables e cepting the pressure !ill affect mercaptan e traction efficiency. &oo :o! an operating pressure fa%ours amine and caustic entrainment in LPG stream. III. TYPICAL OPERATING DATA AS O"SER$ED IN T#E NORMAL RUN OF T#E UNIT (#&1(L-7 77.76 <.DE <.77 74 (#&1(L-4 4E <.8 >il 74.C

LPG flo! (mine flo! #austic flo! .ack pressure

)D0hr )D0hr )D0hr 'g0cm4

- 34 -

C#EMICALS ! CATALYSTS , :nitial fill )D (ppro . #austic le%el of strength initial fill G !t. D<-C<G 6.F of upper LPG )ake up0 Juantity charge out !hen re-d. 9 p.to run !hen design crude #austic (bout 7<G of 9%ery strength do!n initial fill month to 7.CG 2drain upto bottom LG and make up3 (s re-uired to maintain rundo!n LPG >ot in use no! odour at le%el 42min3

Hessel no

#austic <44H7

9thyl tan

mercap-

:. ::. :::.

MODIFICATIONS' "acility to route S5 LPG to #5 LPG unit and %ice-%ersa. "acility to route #5 LPG to S5 LPG Mero 2unit 443 partially. (fter (H1 re%amp, S5LPG make has gone up and no! S5LPG is being treated in 4E 1nit !hich !as earlier treating #5LPG. >o! S5 LPG is treated :n 1nit 44. "ollo!ing changes in operation ha%e been done to achie%e LPG specifications. #austic circulation in e tractor has been stopped due to caustic, carryo%er 8 )D caustic is taken in this column !hich is acting as another pre!ash. +ue to high LPG production. caustic carry o%er continued resulting LPG falling in #u corrosion test. >o! ."A is being taken in this column to !ash the caustic ha;e carried from 44H7.

:H. >ame of the Scheme Scheme for con%ersion of 44#4 to amine absorber

- 35 -

Scheme >o Scheme implemented on +escription of Scheme 5eason for modification

)50PS0D<<04<<7074 (prN<4 #on%ersion of !ater !ash column 44#4 into (mine absorber in cracked LPG )ero +ue to higher LPG generation of around D6-D8 mD0hr, load on 44#7 had increased leading to %ery often amine carryo%er from 44#7.Aater !ash column if con%erted into amine absorber !ould take part of the LPG load and !ould lead result in better e traction of $4S from LPG 7. 44#4 !ill no! be operated as amine !ash column. LPG from "##1 !ould get distributed in 44#7 and 44#4.7< )D0hr of LPG flo! !ould go to 44#4 controlled through 44"5#7D. 4. 44"5#7D !ould be gi%en a set-point of 7< mD0hr. D. (mine flo! through 44#4 !ould be maintained through 44"5#F. &his !ould be gi%en a set point of <.7 )D0hr. E. (mine le%el in 44#4 !ould be maintained by 44L:# 8. &his !ould al!ays remain on auto. C. (mine and LPG le%el interface is maintained in the lo!er half of the column.

/perating :nstructions

- 36 -

&. U-23 $IS"REA ER NAP#T#A MEROX UNIT CAPACITY

&he )ero treating unit for s!eetening the naphtha stream obtained from the %isbreaker unit has been designed to feed 6C,<<< )&0year of naphtha. &he unit shall operate for DD< stream days in a year. FEED SPECIFICATIONS (#&1(L 7< ma D<<< ma <.7E C< 7C< 7<-77< D<<<-E<<< <.77-<.74 C4

+9S:G> $4S !ppm )ercaptan !ppm +ensity at 7C=# +istn. ".P :.P 776

PRODUCT SPOECIFICATIONS

)ero treated naphtha shall meet the follo!ing specifications 2i3 #opper strip corrosion 2 D hours at C<=# 3 2ii3 )ercaptan sulphur !t ppm 76D-64 2iii3 / idation stability minutes.2after in@ection of 1/P >o.C copper deacti%ator3 7 ma . (S&) +-7D<-6C C ma . 1/P DF< min (S&) +-C4C-CC

TYPE OF CATALYST USED

)ero catalyst !s !hich is dispersed in caustic solution is used in the e tractor column <4D-#4 of this treating unit. )ero #atalyst ". is used in the s!eetening 5eactor <4D-57 of the unit. &his is impregnated on acti%ated charcoal bed in the reactor both the catalysts are supplied by 1/P. :nitial charge of catalyst AS is E.< gal. and it is added !hene%er spent caustic is dumped and fresh caustic solution is made up in the e tractor column for one impregnation on the reactor bed. 7.D gal. of catalyst ". is used.

- 37 -

PROCESS DESCRIPTION

Caustic prewash vessel is provided for removal of hydro e! sulphide etc" "or %isbreaker naphtha, both e traction and s!eetening sections are pro%ided. (fter caustic pre!ash naphtha goes to e traction to!er !here partial e traction of mercaptans, to the e tent possible are e tracted. 9 traction is follo!ed by s!eetening in reactor !ith supported mero catalyst bed. (ir re-uirement is met from the common compressor . Post treatment consists of a caustic settler, and a sand filter for remo%ing caustic ha;e. &he treated product re-uires anti-o idant in@ection, since %isbreaker naphtha is a cracked product. DETAILED DESCRIPTION OF P!ID

Hisbreaker naphtha as obtained from Hisbreaker stabiliser bottom is fed to the unit by feed pumps <4D-P7 (B.."lo! control <4D-"5#-D on discharge of pump is cascaded !ith %isbreaker stabiliser bottom le%el control. Hisbreaker naphtha can be di%erted to slops, !hen necessary,do!nstream of <4D-"5#-D. #austic pre!ash %essel <4D-H-7 2 7<<< )) 67<< )) 3 is pro%ided for remo%al of hydrogen sulphide etc. &he %essel is also pro%ided !ith a stainless steel !iremesh blanket at the top to remo%e any caustic entrainment. &here are three inlet no;;les like in other pre!ash %essels. #austic in the %essel is to be changed out as indicated by its strength. &he feed then goes to e tractor column <4D#-7 2 7<<< )) 7DD<< )) 3 and is introduced at the bottom of column !here counter-current contact is made !ith caustic under circulation. 5egenerated caustic from caustic regenerator section is introduced at column top on flo!, control <4D-"5#-8. &hrough the e tractor trays caustic flo!s do!n!ards due to its higher gra%ity. #austic after e traction is sent to caustic regeneration section by maintaining the <4D-#: bottom caustic le%el by <4D-L:#-7. :n the e tractor, mercaptans are partially e tracted to the e tent these are soluble in caustic. (bout E<-6<G mercaptans are normally e tracted. &his !ill %ary !ith the type of feed to %isbreaker and operating conditions of %isbreaker . &he e tracted naphtha then goes to )ero 5eactor <4D-57 2 7E<< )) EC<< )) 3 for s!eetening of une tracted mercaptans. &he reactor consists of a solid bed of acti%ated charcoal impregnated !ith mero catalyst >o.7. / idation air is added to %isbreaker naphtha on flo! control <4D-"5#-7C and mi ed thorougly !ith feed in the air-mi er <4D ) 7 before it goes to reactor. 1niform distribution of feed o%er reactor bed is ensured by the distributor pipe assembly placed inside the reactor. &he collector assembly at the bottom is !rapped !ith Lohnson screen to ensure filtering of reactor bed material from the hydrocarbon stream. "rom the outlet of reactor, caustic remo%al from %isbreaker naphtha is achie%ed in the caustic settler <4DH42 77<< E7<< 3. &he feed to the settler is distributed by a slotted %ertical pipe.
- 38 -

&he treated product from settler is sent to storage %ia a sand filter <4D-HD 2 7E<< D8<< 3 for remo%al of caustic ha;e. &he inlet distributor consists of slotted pipes assembly. Sand is filled from half !ay up the %essel and supported on the packing support pro%ided at that le%el. .elo! the sand packing segmented baffle is pro%ided in front of outlet no;;le* to ensure clear hydrocarbon !ithdra!al from sand filter. &he treated product is sent to storage after the pressure control <4DP#-7F !hich ensures constant back pressure to the unit. &he sand filter is also pro%ided !ith a bypass, for use !hen necessary. Hisbreaker naphtha being a cracked product re-uires to be do;ed !ith o idation inhibitors. 1/P >o.C inhibitor from drums can be transferred to inhibitor melting pot <4D-H6. &hree inhibitor metering pumps <4DP-D(, .B# are pro%ided. <4DP-D( is for in@ecting inhibitor into %isbreaker naphtha, <4DP-D# is for in@ecting to "## gasoline and <4DP-D. is a common spare. :nhibitor is added upstream of <4DP#7F control %al%e !hich ensures constant pressure. "or circulation of reactor caustic as !ell as for !ater !ash and methanol circulation, pumps <4D-P4 (B. are pro%ided. "or impregnation of catalyst, catalyst addition pot <4D-HE and flo! indicators <4D":-7< B <4D":-77 are to be used !hen impregnation is carried out in line !ith standard impregnation procedure. "or acidifying charcoal bed during reimpregnation acetic acid addition pot <4D-HC and eductor <4D-L4 are pro%ided. &he treated and inhibited %isbreaker naphtha !hich is doctor s!eet shall normally be used as a motor gasoline-blending component. :. PRECOMMISSIONING OPERATIONS C#EC ING OF CONSTRUCTION WOR AND "OXING UP OF EQUIPMENT. COMPLETION( INSPECTION

&he follo!ing preliminary operations are to be carried out in order to ensure a trouble free and smooth startup of the unit. #heck that all mechanical !orks of construction ha%e been completed. (ll e-uipments and lines in the unit must be hydraulically tested at pressure depending upon design conditions so that !e can be certain that they !ill stand operating pressures. (fter the hydraulic test, e-uipment are finally inspected for proper internal fittings and fi tures as !ell as cleanliness. #learance are gi%en to bo up e-uipment after final inspection as abo%e. #hecklists are signed off as complete in all respects for indi%idual e-uipment and pipelines. )ake a final blind list indicating !hich blinds are to remain in position and !hich are to be taken out before starting gas-purging operations. 9nsure that all blinds ha%e been installed at the proper sides of %al%es and entered in the list. #heck and ensure that fire fighting and safety e-uipment are readily a%ailable in the unit in good !orking condition. 9nsure that all utility systems and flare release header are in ser%ice and ready for use.
- 39 -

9nsure free mo%ement in the unit area. Get scaffoldings, construction debris tools and tackles etc. remo%ed from the unit area. :solate the unit from other plants and storage tanks at the unit limits !ith block %al%es0blinds for carrying out flushing and purging operations. :solate or remo%e instrument orifice blocks for flushing purposes. II. WATER FLUS#ING OF T#E UNIT

:n preparation for start-up of the unit, !ater flushing of the entire unit has to be carried out to remo%e and !ash out all muck, scales construction debris etc. from e-uipment and lines for the purpose of !ater flushing, the unit can be taken up in con%enient sections as !ell as indi%idual e-uipment-!ise also. $ooking up temporary fire !ater hose connections on e-uipment or lines, thorough flushing of all e-uipment and lines are carried out. (ll the unit pumps are tried out during !ater flushing !ith suitable !ire mesh screens 2 preferably 7<< each 3fitted on to their suction spools to pre%ent them from damages. &he pumps ha%e to be run at least for 4E hours continuously to ensure their free and smooth functioning. #are has to be taken !hile running the pumps not to o%erload their motors, during the !ater flushing operations &heir discharge %al%e ha%e to be suitably throttled to take care of the loads on motor. +uring the pumps running-in period, the suction screen !ill get choked up !ith debris !ashed out into them and they !ill start losing suction. :mmediately the pumps are to be stopped. screens opened up, cleaned and then pumps restarted. &his cleaning operation !ill ha%e to be continued till the suction screens remain clear of all debris and muck at least for 8 hours. /n satisfactory completion of !ater flushing of the unit. (ll the !ater from e-uipment and lines are to be drained out, opening drains and flanges at lo! points. #are should be taken not to pull any %acuum in the e-uipment !hile draining !ater. &hen, thoroughly air blo! the entire unit to remo%e all traces of !ater remaining after !ater !ashing. III. PRESSURE TESTING OF EQUIPMENT ! PIPELINES

Subse-uent to !ater flushing of e-uipment and lines in the unit, a pressure test is carried out !ith !ater to about 7< kg0cm4 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. +uring the test safety %al%e do!nstream flanges are opened up to check holding of safety %al%es. (ny safety %al%e !hich re-uires resetting is remo%ed and sent to !orkshop for repair. Pressure test !ith !ater can be con%eniently carried out by running the feed pump or caustic pump and pressure up the unit by restricting the flo! at the plant outlet till the desired pressure is reached. #are has to be taken during pressure test to isolate e-uipment and piping !hich are designed for lo!er pressure, like e.g. methanol system. &hese can be tested separately at lo!er pressure.
- 40 -

(fter pressure test is satisfactorily completed, drain !ater from system at all lo! point and air blo! it thoroughly to remo%e all moisture. I$. SCREENING AND LOADING OF C#EMICALS

(#&:H(&9+ #$(5#/(L (cti%ated charcoal !hich mero catalyst impregnation !ill be screened properly before it is loaded in the reactor 4D57. Standard (S&) Sie%e >os. 7< and D< screens ha%e to be used and charcoal coarser then >o.7< and fines after >o.D< screen are separated out. &he charcoal thus screened is loaded in 4D57 after isolating it from other e-uipment. :ts top and side man!ays are kept open. :ts inlet distributor pipe assembly has to be kept *#o%ered during loading to pre%ent charcoal entry into the pipe. #harcoal loading is done through a hopper and ad@ustable can%ass chute, !hich e tends to the bottom of the reactor. (s loading progresses, the length of the chute is ad@usted. >o cone formation is to be allo!ed on the charcoal surface in the reactor. :mproper le%eling !ill cause nonuniform distribution of hydrocarbon flo! through the charcoal bed. Personnel must !ear dust masks co%ering their noses and mouths to pre%ent inhalation of charcoal dust, !hile loading for le%eling inside the reactor, the person entering must !ear a fresh air mask. Ahile loading, it has to be ensured that the *bottom Lohnson screen collector :s fully submerged in the charcoal by physical checking, from the bottom man!ay. &he charcoal loading is continued till the inlet distributor pipe is about F<< mm from the charcoal bed. "inal le%eling is done entering the reactor top !ith protecti%e e-uipment. 5ecord of -uantity of charcoal loaded in the reactor is kept for reference. &he loading hopper and can%as chute are remo%ed after loading, the co%er on distributor pipe is taken out and the top ma!ay of the reactor is bo ed up tight. S(>+ #heck the internals of sand filter 4D-HD for proper fittings and support for sand *bed, #heck also it is !iped clean from inside sand screened to the specification of 8-76 (S&) >os. is then loaded to a height of 7.E meters in the filter. &he surface is le%elled properly and then the %essel is bo ed up finally. $. PRESSURE TEST FOR TIG#TENESS

Ahen all chemicals ha%e been loaded as re-uired and all man!ays, flanges, etc bo ed up the unit is ready for impregnation of catalyst on charcoal bed. .efore impregnation of catalyst, it is preferable to test the unit for tightness of flanges, man!ays. etc. under air pressure. #ompressed air e 47 #: (, . can be used for pressuring up the unit to about 7< kg0cm 4* pressure. (fter the unit is pressured up. check all flanges man!ays, etc for tightness !ith soap solution. &ighten as re-uired. Ahen pressure test is o%er release the pressure gradually in order not to disturb the bed of charcoal. $I. IMPREGNATION OF CATALYST ON REACTOR 23-R1
- 41 -

(fter the reactor is filled !ith charcoal to the re-uired le%el and bo ed up proceed to impregnate charcoal !ith )ero catalyst ". as detailed in the follo!ing steps. "ill the reactor !ith +) !ater being careful not to add so much !ater as to float charcoal out of reactor.&o ensure this. reactor top man!ay can be kept open. /nce le%el is ensured man!ay can be kept in closed position !ithout bolting to enable inspection of bed after impregnation. Stop + ) !ater supply and line up reactor bottom to reach circulation pump 4D-P4 (. . and establish from bottom of bed to top of bed. 9stimate the amount of !ater in the system i. e. reactor, lines etc. :f !ater is charged from a tank, this can be estimated con%eniently from tank dips. 9stimate should take into account piping, dead spaces etc. &he total -uantity !ill be about 6-7 )D. #alculate the amount of ammonia re-uired to raise the concentration of !ater to a <.4G !t solution of ammonia. &he -uantity of ammonia re-uired !ill be about 74-7E kgs. Aith !ater in circulation, in@ect the desired amount of ammonia into the !ater upstream of suction line to pump 4D-P4 (. .. (mmonia is in@eted from a cylinder mounted on a suitable !eighscale so that the -uantity of ammonia in@ection can be controlled. (d@ust ammonia in@ection rate in such a !ay that the amount needed !ill be introduced during the time it takes to pump the entire !ater in%entory through this system t!iceO !ith pump this !ould takes D to E hrs and hence ad@ust ammonia in@ection to last this period. Ahen ammonia concentration is uniform in the system. fill the catalyst mi drum !ith ammonia !ater. (dd the content of D bottles of 4.C gallons each of mero ". catalyst. &his contains 7.C kg of acti%e ingredient. )i ammonia !ater and catalyst solution thoroughly using an air sparger. :n the catalyst mi drum do not e ceed 8<G le%el. Aith !ater still circulating from the bottom of the reactor to top, educt the catalystammonia !ater into the system at a rate of appro imately E liters per minute. (fter emptying the mi -drum, flush it se%eral times !ith (mmonia !ater and educt the !ater into the reactor to get all of the residual catalyst into the reactor. #ontinue circulation of ammonia !ater for one more hour after all catalyst has been educted. "inally drain all !ater from the system. &he catalyst is no! ready for alkali;ing !ith a 7<=.e solution of caustic. &ransfer caustic of this strength to the settler 4DH4 to about D<G of its %olume. Start caustic circulation !ith pump 4D-P4 (0. through the reactor 4D-57. :nitially keeping the drain %al%e open, remo%e all the free !ater till caustic appears at the drain. #lose off the drain and continue circulation at the ma imum discharge rate for about t!o hours. :f necessary. take additional caustic from storage tank into settler 4D-H4. Stop circulation after t!o hours and the reactor is no! ready after impregnation to recei%e hydrocarbon feed for s!eetening.
- 42 -

$II.

C#ARGING OF C#EMICALS

#austic re-uirements of the unit is met from the storage facility a%ailable in the kerosene mero section. "resh caustic of 46.C G.e strength is recei%ed in storage tanks 47 &: B &4 and diluted !ith demineralised !ater to the desired strength. 7<o.e caustic is charged into the pre!ash %essel 4D-H7 till a !orking le%el is established in 4D-H7. 4<=.e caustic from the disulphide separator 4E-HE of the cracked LPG )ero 1nit is charged to the e tractor column 4D-#7 top through a 7704I line by the transfer pump at cracked LPG )ero 1nit. &his caustic drop after e traction of mercaptans is sent back to the regeneration section on le%el control from the bottom of e tractor column. &o begin !ith 4<=.e caustic is transferred to the disulphide separator from kero mero unit to establish sufficient le%el for subse-uent transfer to other mero sections. START-UP PROCEDURE

:t is assumed that the mero system is fully lined up for startup. Proceed to start-up the unit as follo!s ,Ahen %isbreaker naphtha becomes a%ailable commission the charge pumps 4DP7 (0. and slo!ly introduce naphtha into the pre!ash %essel 4D-H7 and fill it up. Let it pass through the e tractor and then the reactor and caustic settler. "inally, pass naphtha through the sand filter 4D-HD to the rundo!n line to storage. Hent out all air before filling the %essels. #ommission the pressure controller 4D-P#-7F to ha%e the re-uired back pressure in the system. )aintain proper le%els of interface in 4D-H7 and 4D-#7.#ommission the bottom 4DL#7 of 4D-#7. Start air in@ection thro* mi er 4D )K7. &ake the flo! on control 4D-"5#7C and set the flo! rate to the re-uirement 2D< kgs0hr.3 of mercaptan sulphur in the feed. 4D P#-7F should be set such that all air in@ected is in hydrocarbon solution. :n a freshly charged mero 5eactor, no caustic circulation !ill be needed on the initial start-up period. $ence it is enough to pass the feed through the reactor, !ith air mi ing as already mentioned abo%e. Ahen catalyst acti%ity declines o%er a period of time, resaturation !ith caustic circulation is resorted to. #austic carried o%er along!ith naphtha is settled in 4D-H4 and drained back to the circulating pump suction. (ny traces of caustic ha;e still remaining is remo%ed in the sand filter 4D-HD and the treated naphtha is routed to storage from the sand filter. #ommissioning the inhibitor in@ection facility, the metering pump 4D-PD(0. is started to in@ect the measured -uantity of inhibitor into the naphtha stream going out to storage. &he present in@ection rate is 8< to F< ppm so as to get a minimum induction period of D6< minimum.
- 43 -

:nitially, the product stream is routed to the slop tank till satisfactory results are obtained consistently for about 4 hours. &hen naphtha can be routed to the regular storage tanks. Set the feed rate to normal consistent !ith other control systems parameters. REACTOR "ED WATER WAS#ING ! CATALYST REIMPREGNATION

/%er a period of time, catalyst in the reactor bed loses its acti%ity and e%en !etting !ith fresh caustic circulation does not help in restoring the acti%ity and the product continued to go off specifications. &hen the charcoal bed has to be hot !ater !ashed to remo%e the organic deposits on its pores. Aashing !ill bring back the acti%ity of the catalyst for reaction again. (s the loss of acti%ity by deposits on charcoal surface occurs gradually the !ater !ashing operation can be planned con%eniently &he !ater used should be dust free and free from suspended matter. hardness, salts and acti%e chlorine. +) Aater is therefore, used in our plant for this purpose. Aater !ashing procedure is as follo!s , Stop air in@ection and hydrocarbon charge to the reactor 4D 57. Pump out all naphtha from 4D 57 under steam pressure. Steam out the reactor for about an hour. #ommission !ater heater 4D L: and start introducing hot !ater into reactor at a temperature of 8C - FC=# at a rate of 8 gallons0minute for 7<< cubic feet of charcoal bed i. e. about D.C )D0hr. "ill up the reactor and drain !ater to se!er at the same rate as filling. &he effluent from reactor bottom !ill be dark bro!n and foaming in the beginning. &his !ill change and become colourless gradually !hen !ater !ashing progresses. Ahen the drain !ater is clean and clear. &he !ashing of the reactor bed can be stopped. &hen blo! out as much !ater as possible from the reactor !ith steam gi%en to it from the top. #ontinue steam blo!ing for another half an hour to remo%e from the charcoal %oids as much residual hea%y oil as possible. Stop steam to reactor and block of !ater heater. .lanket the reactor !ith nitrogen and blo! it !ith >4 gas for an hour or so till there is no !ater dripping from the bottom drain. >e t alkali;e the reactor bed !ith 7< o.e caustic solution and then return the unit back to normal operations, as detailed under IStart-up procedure.I I. CATALYST REIMPREGNATION

#atalyst reimpregnation step is necessary only !hen hot !ater !ashing, higher feed temperature, stronger caustic reduced feed rates etc. do not help in mercaptan o idation and the product remains off-spec. Gap bet!een one reimpregnation and another !ill depend on proper pre!ashing, feed mercaptan content, crude etc. Period may %ary from three months to one year depending on feed -uality. +etailed steps for reimpregnation are as gi%en belo!,

- 44 -

"ollo! the steps C.7.7 to C.7.E gi%en under I5eactor .ed Aater !ashingI, e cepting the steaming of reactor. "ill up the reactor !ith hot !ater. &hen stop !ater and steam flo! to the !ater heater by blocking off the %al%es. Line up reactor bottom drain line to caustic circulation pump 4D P4 (0. and flush out the lines free of caustic into the spent caustic disposal system. #lose the reactor outlet %al%e and fill it up !ith hot !ater again. Start hot !ater circulation from reactor top to bottom, regulating !ater temperature !ith steam around C<-7<=#. 'eep both the drain line and reactor outlet lined up to the circulating pump. &ake about 4< liters of glacial acetic acid in the addition pot 4D-HC and close the lid of 4D- HC. 9duct the acid from 4D-HC into the circulating !ater !ith the help of the D0EI globe %al%e on pump 4D-P4 (0. discharge. 9ductor 4D-L4 takes suction from the acetic acid addition pot 4D-HC. 9duct the acid to the circulating !ater to reactor o%er a period of C-7< minutes. #irculate the acidified !ater for an hour and check its P$ at the pump 4D-P4 (0. suction. :f P$ is more than 6.C another 4< litres of acetic acid !ill ha%e to be educted till the circulating !ater P$ is 6.C or less. Stop !ater circulationO introduce steam into the reactor and remo%e all !ater from the bottom drain. 'eep steam blo!ing for another half an hour and displace all traces of residual oils from charcoal %oids. Stop steam to reactor and blo! it !ith air till !ater drips from its drain stop. &hen follo! the steps gi%en under I:mpregnation of catalystI under D.6. 1nit can be returned to its normal duty as soon as reimpregnation of catalyst is o%er. S#UTDOWN -PROCEDURE

"or planned shutdo!n for inspection of e-uipment and maintenance !ork in the unit, follo! the se-uence of operations gi%en belo!, :nform all concerned of intention to shutdo!n the unit. Shut off air in@ection block %al%e to the mi er )M7. Shut off naphtha charge pump 4DP7(0. to the pre!ash %essel 4D H7. #lose off the pressure controller 4DP#-7F at the battery limit. Shut off anti-o idant in@ection pump 4DPD(0. to the naphtha stream before 4D P#-7F. Stop caustic circulation through the e tractor 4D#7 and reactor 4D 57. Pump out caustic from 4D #7, 4D 57, 4D H4 and 4D HD to spent caustic disposal system. Pump out all caustic from 4D H7 bottom into the spent caustic drainage system. Pump out hydrocarbons remaining in the %essels to the slop tank !ith circulation pump 4D P4 (0..
- 45 -

"lush out reactor 4D 57 !ith hot !ater thoroughly and drain off all !ater. :solate all indi%idual e-uipment by blinds as re-uired for maintenance. Steam and !ater !ash them thoroughly till they are hydrocarbons and chemicals free. )aintain an upto date blind list of unit e-uipment. "ollo! detailed instructions that !ill be gi%en at the time of shutdo!n for preparing e-uipment and lines gas free and for maintenance. 9ntry to the %essels should be gi%en only after ensuring complete isolation by blinds, making gas free and free of chemicals. (lso, it must be ensured that the %essels are !ell %entilated and are safe to enter. Gas test must be taken before issuing clearance for entry into a %essel Safety e-uipments recommended must be !orn by personnel entering %essels !hich pre%iously contained caustic and other chemicals. EMERGENCIES

9mergencies result out of e-uipment failures and from interruption of utilities. /perating personnel must be thoroughly familiar !ith the emergency procedures so that -uick actions can be taken in such situations. >ature and degree of an emergency %aries from time to time. $ence, good @udgement and discretion should be e ercised to tackle any emergency. I. ELECTRIC POWER FAILURE

:f it is a general failure, naphtha feed to the unit !ill be lost and all unit pumps !ill stop. 1nit !ill ha%e to be immediately shutdo!n. blocking off air in@ection to mi er )M7. #lose off the pressure controller at battery limit and hold the system pressure. Shut off the discharge %al%e of pumps. $old the le%els in the %essels. Start up the unit again follo!ing standard procedure. !hen po!er supply is restored. II. STEAM FAILURE

Local steam failure !ill not effect the unit immediately :f the naphtha feed supply from %isbreaker is affected then unit !ill ha%e to be shutdo!n and kept standby till the feed naphtha is a%ailable again. III. INSTRUMENT AIR FAILURE

(ll control %al%es !ill operate to fail safe position i.e. they !ill close. Shut off the air to the reactor by the block %al%e to the mi er )M7. $old the pressure in the system and monitor all le%els till air supply is restored to the instruments. Start-up the unit as per normal procedure and bring it back on stream. I$. COOLING WATER FAILURE

( total !ater failure !ill affect feed supply to the unit as !ell as unit pumps. $ence. unit !ill ha%e to be shut do!n immediately. Stop the pumps. .lock off pressure
- 46 -

#ontrollers and hold system pressure. )aintain all le%els in unit %essels. Ahen cooling !ater becomes a%ailable, start up the unit, as per normal procedure. "or a short duration, process air failure !ill not affect the treated naphtha -uality. .ut the mercaptan con%ersion efficiency drops off rapidly !ith no air for o idation. $ence the product !ill ha%e to be stopped as soon as it becomes doctor positi%e. Shut off air in@ection block %al%e to mi er )M7 immediately on air failure. OPERATING $ARIA"LES

#austic solutions used in pre!ash %essel 4D H7 and reactor 4D 57 become spent e%entually and mercaptan e traction !ill suffer. $ence, periodically, part of the caustic !ill ha%e to be replaced !ith fresh stock. #austic concentration in the solution for e tracting lighter mercaptans in 4D #7 must be 4<=.e. #atalyst concentration in caustic should be 7<< ppm. /perating pressure should be about 8 kg0cm4 to keep the air in@ected dissol%ed in hydrocarbon. Lo!er pressure results in %aporisation and caustic entrainment. &oo little air !ill result in incomplete o idation of mercaptans to disulphides. (bout D< cu. feet of free air is re-uired for each lb of mercaptans sulphur to be o idised. #atalyst acti%ity in the reactor bed is increased by resaturation !ith 7<=.e caustic circulation freshly taken and circulated through the bed. $ot !ater !ashing and reimpregnation !ith catalyst are further steps to restore the acti%ity of the catalyst. (cid oils upto 8-74G in caustic solution !ill increase solubility of mercaptans in caustic. $4S and naphthenic acid from feed naphtha must be fully remo%ed in the pre!ash %essel 4D H7. /ther!ise o idation reaction !ill be suppressed in the reactor. >aphthenic acid may gi%e rise to emulsion problems. I. T)*+,a- O*e.a/+0g Da/a ' (#&1(L )D0hr 7<.C >)D0hr 4C E< 7.7 4.E to E.< D.< to 6.< 4 to 4.C D<-DC

+9S:G> "eed flo! (ir rate

#austic #irculation rate )D0hr "eed temperature, =#

- 47 -

 Sr

C#EMICALS ! CATALYSTS Hessel >o. 4DH7 4D57 (mmonia 4D57 (cetic acid 4D57 1/P >o.C o idation inhibitor 1/P copper deacti%ato r #harcoal 4D57 Sand 4DHD #atalyst )ero reagent ". 4D57 :nitial fill,)D 4.E 7.C 74-7E kg (bout 7< drums (bout D drums 6.< 4.4 (ppro . le%el of #austic initial fill strength G!t D<-C<G of 6.F upper LG 5efer caustic 6.F tank calibration chart )ake up 0 change out Juantity !hen re-uired Ahen caustic strength to (bout 7<G of initial fill 7.CG 2drain up to bottom LG B make up3 #irculate caustic once in 7C )D F days. #austic good for about C circulations Some -uantity re-uired during each reimpregnation (bout 4< litres for each reimpregnation 5ate of in@ection 76< cc0hr 5ate of in@ection 7<<< ##0hr of mi ture of 1/P >o C B deacti%ator in the ratio of 7,<.D4 7.C gal for impregnation each 9 pected duration !ith design crude 9%ery month /nce in EC days (bout once in E months at design throughput (bout once in E months at design throughput 7< drums good for 6 months D drums good for si months (bout once in E months at design throughput

7.C gal for initial impreg nation

- 49 -

1. U-2% CRAC ED LPG MEROX UNIT CAPACITY

#racked LPG )ero unit is designed to process 7,EC,<<< )&0Kear of LPG from #atalystic #racking 1nit !ith an on stream days DEC per year. FEED SPECIFICATIONS - ? 7G 2)ol3 - ? 47<< APP) - D<< APP) 2)a 3

#C 6 material $4S 5S$-S

PRODUCT SPECIFICATIONS

LPG P5/+1#&, &otal sulphur - ? 7C APP) 5S$-S - ? C APP) #opper #orrosion - >ot !orse than $4S free feed.

TYPE OF CATALYST USED

&he )ero #atalyst used in the e traction section of this unit is 1/P )ero AS. :t is a replacement for the original con%entional po!dered )ero 5eagent >o.4. )ero AS is an a-ueous solution of the reagent ha%ing e-ui%alent catalytic acti%ity and stability as mero 5eagent >o.4. (lthough it is not truly soluble in !ater, it has got considerable dispersibility in caustic solution. :t is packed in polythene bottles !ith 7 kg. of acti%e ingredient in each bottle of D.8 litters capacity. #atalyst is added to the circulating caustic going to regeneration section. &he initial in%entory in a process unit is recommended at 7<< PP) 2by !t.3 or appro imately 7 bottle per E )D of caustic soda and up to C times this concentration in units treating high se%erity "## gasoline. /ne distinguished characteristic of this )ero #atalyst leads to a simple control of unit operation. :f mercaptans or e cessi%e amounts of acid contaminants such as sulfides are absent. ( medium containing appro imately 7<< APP) )ero catalyst imparts a deep blue color. $o!e%er should mercaptan be added, the solution !ill become deep green. :n this comple state, the catalyst e hibits a considerably greater ability to remain suspended. :f the mercaptans in this green mero catalyst medium !ere o idi;ed, the blue color !ould reappear &his phenomenon can, be obser%ed in the shake test !hich is an e tremely useful parameter in e%aluating the process.

- 50 -

PROCESS DESCRIPTION

&$9/5K /" )95/M &59(&)9>& /" #5(#'9+ LPG, &he e traction mode of )ero Process is for the treatment of light hydrocarbons in LPG and light naphtha streams. :t is designed to reduce the total sulfur content by e tracting the mercaptan compounds in these streams. &he e tracted mercaptan compounds can be effecti%ely remo%ed after being o idi;ed to disulfide oils. &he $ydrocarbon stream is contacted !ith caustic solution in an e tractor. 9 tracted mercaptans are then o idi;ed and separated from the caustic. &hus the )ero process is easily described in t!o parts, )95#(P&(> 9M&5#&:/> )ercaptans present in the LPG are readily dissol%ed in the caustic solution !hen e tracted by means of a high efficiency, counter flo! e tractor. (s the hydrocarbon and caustic are intimately contacted, the mercaptans combine chemically !ith the sodium hydro ide molecules. 5S$ 6 >a/$ ?-8 >aS5 6 $4/ Since the reaction is re%ersible, the sodium mercaptide must be remo%ed from the caustic solution from time to time. &he 1/P designed counter amount e tractor pro%ides the effecti%e e traction of mercaptans in to the caustic solution and its remo%al from cracked LPG. )95/M #(1S&:# 59G9>95(&:/> #austic regeneration is for the remo%al of sufficient mercaptides from the rich caustic solution to allo! the reuse of this caustic solution to continuously affect the desired mercaptan remo%al from the hydrocarbon stream. Sodium mercaptides in the rich caustic are readily o idi;ed to disulfide in the presence of o ygen and enough )ero catalyst. Sodium hydro ide reliberated. &his is represented as, )ero >aS5 6 70E <4 6 704 $4/ -------8 704 5SS5 6 >a/$ #atalyst &his is an irre%ersible reaction. &he disulfide oil produced is essentially in soluble in the caustic solution and thus allo! it to be gra%ity separated from the regenerated caustic before the lean caustic is allo!ed to return to the e tractor. &he composite reaction is 5S$ 6 704 <4 -8
7

04 5SS5 6 $4/

&he composite reaction does not consume caustic, if only the mercaptans are e tracted. $o!e%er the other e tractable compounds such as $ 4S, #<4, #/s do not allo! full reco%ery of caustic. Pretreatment of hydrocarbon stream becomes
- 51 -

necessary to remo%e ma imum amount of $ 4S. &his is accomplished by (mine absorption follo!ed by !ashing !ith dilute caustic of 7G by !t. Post treatment is normally for the remo%al of entrained caustic solution due to its corrosi%e nature to protect do!n stream process e-uipment and to meet product specification. DETAILED DESCRIPTION OF P ! I D

&he cracked LPG from "## gas concentration stabili;er o%erhead is recei%ed in amine scrubber 4E#7 27E<<< mm 7FC<<3 ha%ing 77 absorption trays Lean amine from (mine 5egeneration unit located in Sulphur plant area after regeneration is recei%ed in surge drums <4E H7 2F<< mm D7<< mm3. &he entry of amine into surge drum is controlled by <4E L# 48 to maintain le%el in the %essel. &he drum is maintained under pressure by blanketing !ith s!eet fuel gas as a%ailable from fuel gas amine absorption unit &he pressure controller <4E P:# D7 is a split range controller !ith t!o control %al%es one on the fuel gas line and one on the flare line. (mine from surge drum is pumped to <4E #7 by pumps <4E P4 ( B . on flo! control <4E "5#-C. &he pump also deli%ers amine to amine absorber of unit <44 for S5 LPG. &here is also a minimum from bypass line from discharge to suction of the amine pumps for use !hen pumped out -uantity is less. :n <4E #7 amine enters the top of the column and LPG is introduced at the bottom. #ounter-current absorption takes place as LPG rises up through the perforated trays pro%ided in the column. 5ich amine from column bottom is sent to (mine 5egeneration unit under column pressure. &he flo! of rich amine is controlled to maintain column bottom le%el by <4E Ll# E. LPG from top of <4E #7 goes to caustic pre!ash %essel <4E H7 on flo! control <4E "5#-7, !hich is cascaded to "## gas conc. stabili;er o%erhead %essel le%el control. :n order to keep good e traction efficiency at lo! throughputs or to ha%e good control on flo! in case flo! of LPG is unsteady, part of LPG from e tractor can be circulated back to "## stabili;er o%erhead %essel, using <4E "5# 47 for o%erall LPG flo! control. LPG to caustic pre!ash %essel 276<< 67<<3 can be distributed into the %essel using one of the three distributors pro%ided. >ormally the one at the bottom is used. #austic in the %essel is changed out !hene%er caustic strength comes do!n belo! specified le%el. &he %essel is pro%ided !ith an SS !ire mesh blanket to minimi;e caustic mist carryo%er. LPG after remo%al of hydrogen sulfide in absorber and pre!ash %essel goes to e traction column <4E #4 27E<< 7DD<<3 for e traction of mercaptans. &he e tractor is fitted !ith 7 trays of perforated tray type. 5egenerated caustic from caustic regeneration section enters the top of column on flo! control <4E "5#-F. 9 traction of mercaptans takes place in the column and e tracted LPG from top of column is sent to caustic settler <4E H4 27E<< C6<<3. 5ich caustic from bottom of e tractor goes to caustic regeneration section. &he flo! of rich caustic is controlled to maintain bottom le%el by <4E Ll# 8. LPG is introduced into the caustic settler through a slotted %ertical pipe distributor. &he caustic settling do!n in settler can also be di%erted to caustic regeneration
- 52 -

section. LPG from top of settler is sent to storage. .ack pressure controller <4E P# 77 on run-do!n line maintains sufficient and constant back pressure in the unit. :n@ection of ethyl mercaptan to maintain odor le%el is also done on the run-do!n line. )ercaptan storage and pumping facility is common for straight run LPG and cracked LPG. &he e tractor caustic from straight run LPG, %isbreaker naphtha and cracked LPG are combined together for caustic regeneration. &he combined caustic goes to caustic heater <4E 97 !here caustic temperature can be increased by about 7<=# or so to fa%or caustic regeneration reactions. &he heating is !ith steam and to a%oid caustic embrittlement it may be necessary to operate !ith a minimum back pressure on steam-side to ensure lo!er condensation temperature. (ir re-uired for o idation is introduced into caustic at the outlet of heater. <4E "5#-7D, <4E "5#-7E, B <4C "5#-7C ha%e been pro%ided on the airline to regulate air flo!s to suit caustic flo!s from three mero units. ( special spring loaded check %al%e mounted in the airline ensures proper mi ing of air and caustic going to o idi;e. )ero catalyst as necessary is in@ected into caustic going to o idi;er at a point upstream of heater. "or preparation of catalyst slurry B in@ection, catalyst addition pot <4E H6 2EC< F<<3 and necessary hose connections are pro%ided. #austic-air mi ture enters o idi;er <4E HD 27<< 7<<<3 at the bottom through a slotted hori;ontal pipe distributor. &he %essel is filled !ith 7 704I carbon rasching rings upto the top co%er. &he bed of carbon rasching rings packing pro%ides sufficient contact surface necessary for o idation of mercaptides in caustic. &he caustic containing mercaptides, !hich are o idi;ed to disulfides, lea%es at the top of %essel and goes to disulfide separator. &he disulfides in caustic after o idi;er are insoluble in caustic and hence separate out !hen caustic is gi%en enough settling time. &he disulfide separator %essel <4E HE 276<< 6C<< B EC< 78<<3 is pro%ided in line to separate out disulfide oil and to safely %ent out unreacted air !hich !ill separate in the %essel. &his is a hori;ontal %essel pro%ided !ith anthracite packing as coalescing medium to separate out disulfide oil. ( small cylindrical %essel kno!n as *skim pot* packed !ith steel rasching rings in its top portion is mounted on one side of the %essel. &he separated air !ill contain traces of disulfide %apor mercaptans, and traces of hydrocarbon. .ecause of its composition, a possibility e ists for destructi%e internal combustion. &he steel rasching ring packing ensures relati%ely short residence time for the %apors and also pre%ents propagation of flame should it e%er occur. .esides the steel rings reduce the possibility of ignition occurring due to static discharge. &he regenerated caustic enters the skim pot of separator at a point @ust belo! the ring packing, through a hori;ontal slotted pipe distributor. #austic le%el is maintained in the skim pot by <4E L:# 4C by controlling the flo! rate of incoming caustic to regeneration section !hich is achie%ed by controlling either one of e tractor caustic streamsO coming from S5 LPG, #racked LPG or H. naphtha mero es. #austic flo!s across the %essel through the anthracite packing to effect separation of disulfide from caustic. &he anthracite packing in the form of fine po!der is held
- 53 -

bet!een t!o support rings !hich hold !iremesh screens supported on grating bars. "or searing of the supporting grids, nylon ropes are used. +isulfide oil !hich separates out !hile passing through the anthracite packing floats on top of caustic "rom time to time as indicated by le%el disulfide oil shall be pumped out to slop tanks. "rom the disulfide outlet no;;le there is a line connecting to skim pot %ent off any air, !hich does not separate in the skim pot. Ahile pumping out disulfide oil from %essel. :t is ad%isable to check the le%el of caustic in skim pot and ensure that the le%el is sufficiently belo! the %ent line @oining from disulfide outlet line. /ther!ise there is a chance of draining out caustic along!ith disulfide oil. &he #austic from the bottom of the separator is circulated back to e tractor column by caustic circulating pumps <4E P7 (B.. &he caustic streams to e tractor columns are all under flo! control in the respecti%e mero units. (s regulating one of the rich caustic streams from e tractors controls the caustic le%el in separator, that particular e tractor !ill be !ithout any bottom le%el control. $ence the e tractor le%el should be !atched carefully and if necessary maintain a slightly higher le%el to take care of surges in hydrocarbon le%el !hich !ould upset the column bottom le%el. :f the caustic flo! to o idi;er tends to fluctuate due to hydrocarbon surges. :t is ad%isable to commission the hydrocarbon recycle stream at the outlet of e tractors in order to hold steady flo! to e tractor and %ariable flo! on to recycle streams. &he recycling stream facility is pro%ided in S5 LPG and cracked LPG mero e tractors. :f necessary fresh caustic can be added into the system. &he air, etc. from the top of separator is safely disposed off either by %enting it at a high point or by di%erting into a nearby firebo . &he back pressure controller <4E P# 4E on the %ent line ensures necessary B constant back pressure in the caustic regeneration section. &here is an o ygen analy;er <4E (5 44 placed on the line to monitor continuously the composition of gas and should it fall in the combustible range, &his !ill acti%ate the solenoid %al%e trip system placed on the air-line to o idi;er. &hus cutting-off air supply to o idi;er. &he %ent gas can be diluted !ith fuel gas to reduce o ygen concentration. <4E ": 46 on fuel gas line indicates locally the flo! rate of gas !hich can be ad@usted depending on the %ent gas composition. &his !ill support combustion in the firebo . &he %ent gas is lined up to <7F "7 fire bo . &!o flame arrestors are pro%ided upstream of fire bo entry. /ne of them shall be lined up. :f a firebo is not a%ailable, the gas can be %ented to atmosphere %ia %ent tank <4E HC 2EC< 78<<3 e hausting the material at a high point. "uel gas addition is to be stopped in this case. &he %ent tank is filled !ith steel rasching rings in its top portion on a suitable support. (ny condensate collection in the %essel is drained to se!er automatially by gooseneck drain piping. L:S& /" P(#':>GS 273 / idi;er -7704I carbon 5asching rings 27<<< mm height3 243 4E-H-E +ome -7I steel 5asching rings
- 54 -

4E-H-E $ori;ontal portion 2D3 Hent tank >/&9 ,books.

-E to 8 mesh anthracite coal -7I steel 5asching rings

&he packing details should be checked !ith 1./.P original pro@ect

PRECOMMISSIONING OPERATION

#hecking completion of construction !orks, inspection and bo ing of e-uipment. &he follo!ing preliminary checks should be carried out to ensure a successful startup of the unit. #heck that all the mechanical !orks of construction ha%e been completed as per pro@ect book. #heck the entire erection of the unit, e-uipment and lines and compare !ith the Process and :nstrumentation diagrams and any discrepancies should be pointed out and corrected. Scaffolding, debris, tools and other unnecessary construction material should be remo%ed from unit areas. )ake a final list of blinds !hich should be in position or taken out before starting purging operations. )ake sure all blinds ha%e been installed at the proper sides of %al%es and signed off in the list. #heck and ensure "ire-fighting and safety e-uipment is in place and in good !orking condition. 9nsure all utility systems and flare release header is in ser%ice and ready for use. :solate the unit from other plants and tanks at the unit limits !ith block %al%es. 'eep the fuel gas and flare header isolated from the unit pending purging operations. :solate or remo%e orifice blocks of all flo! meters for flushing purposes. A(&95 "L1S$:>G /" &$9 1>:& , Aater flushing of the unit is meant for thorough cleaning of e-uipment internals, and entire pipingO so that all muck, scale and construction debris are remo%ed completely. Aater supply can be taken by temporary hoses from the fire hydrant systems. &he unit can be con%eniently di%ided into small sections and the flushing operations are to be carried out. (ll pumps suction screens should be fitted !ith fine mesh !ires during the flushing operations to protect the pumps* internals. &he follo!ing precautions are %ery important during flushing out period.

- 55 -

:solate all instruments, disconnect the lead lines and flush thoroughly each lead line. +rop control %al%es and flush through the inlet, outlet and bypass lines thoroughly. +isconnect pumps* suction flangesO keep tin sheet to pre%ent !ater getting in to the pumpsO open suction strainer flanges, pull out the strainer and flush each suction line to outside thoroughly. &hen only !e can make up the pumps suction flanges and run the pumps for further effecti%e flushing. Ahile running the pumpsO the fine strainer gets choked -uite oftenO and needs fre-uent cleaning. &hese fine strainers can be totally remo%ed only after cleaning fre-uency comes do!n to once in 8 to 7< hours. Ahile flushing the entire system, make sure that all lo! point bleeders are pro%ed clean. P59SS159 &9S& /" 9J1:P)9>& (>+ L:>9S &he cracked LPG unit contains t!o sections. &he LPG treatment section operates at 7C to 76 kg0cm4 pressure, !hereas the 5egeneration section operates at C kg0cm4. &he pressure testing of these t!o sections should be done independently to check for leak and for rectifying the same. >/&9 ,-#austic regeneration being common to S5 LPG and H. >aphtha )ero 1nits in addition to #5 LPG )ero 1nit, it depends upon !hich )ero 1nit is being commissioned first. >aturally the first unit to be commissioned !ill be S5 LPGO so also all the precommissioning and commissioning acti%ities of caustic. 5egeneration Section !ill ha%e to be done at this time. &he procedural details are noted belo!, P59SS159 &9S& /" )95/M &59(&)9>& S9#&:/> &he high-pressure section consists of (mine (bsorber, caustic pre!ash, )ero e tractor, caustic settler and the %arious connected high-pressure lines and pumps. &his system !ill be pressure tested after complete isolation from 5egeneration Section !ith !ater supply from 7F-P-7E(0.0#. "or this purpose LPG inlet to (mine absorber and its outlet after pressure controller are isolated by block %al%es. 5ich amine and rich caustic outlets from 4E-#-7, pre!ash %essel H7 and 4E#-4 must also be blocked off. :nitial filling of the )ero treatment section can be done from fire hydrant !ater !ith a temporary hose connection. "ill up the entire system and e-uipment !ith !ater and displace air completely. Pressuri;ing the system can then be done by taking .oiler feed !ater supply from 7F-P-7E(0.0#. Slo!ly raise the system pressure up to 78 to 4< kg0cm4. #heck for leaks in the entire high-pressure section and rectify the same. /ne or t!o bleeders can be kept slightly open so that .oiler
- 56 -

feed !ater pump !ill ha%e some positi%e discharge. &he amine surge drum test pressure !ill be around 7 to 7.C kg0cm4 only. So this needs pressure testing separately from high-pressure section and can be done independently by initially filling the %essel !ith !ater and then pressuring !ith hydraulic pumping. (fter pressure test fuel gas backing in to this %essel should be done by separate hose connection. (fter successful completion of pressure testing, depressuri;e the section to around <.4 kg0cm4 !ater pressure. >o! pullout all blinds in the unit as preparatory step for unit startup and keep system isolated by block %al%es only. #ut in fuel gas or take small -uantity of LPG into the system and let it e%aporate. Slo!ly the system !ater should be totally drained out under fuel gas pressure. P59SS159 &9S& /" 59G9>95(&:/> S9#&:/> &his section can be pressure tested !ith ser%ice air up to C kg0cm4. &he caustic heater, o idi;er, disulfide separator and connecting lines and e-uipment are sub@ected to this pressure. Aith soap solution check for leaks and rectify the same. &hen depressuri;e the regeneration section to atmosphere. :n this section there is no need to displace air because later on air !ill be in@ected in to this system as per process needs. #$(5G:>G /" #$9):#(LS (fter pressuring up the unit !ith fuel gas, and total draining of !ater inlet %al%e to the scrubber #7 is blocked off. 9nsure that +9( inlet and outlet from #7 are also blocked off. Similarly, ensure that caustic charge line to H7 and its e it as !ell as )ero caustic inlet to e tractor #4 are all shut off. Prepare 4<=.e caustic solution in the storage tank pro%ided and transfer to disulfide separator <4E-HE. Aith a good le%el in HE, start circulation pump <4E-P7(0. and establish a le%el in LPG e tractor 4E-#-4. &hen line up the pump P7(0. for circulating caustic to e tractor #4, through bottom L:# to the caustic heater <4E-97. / idi;er <4E-HD and back to disulfide separator <4E-HE. (d@ust the circulation on "5# control at the stipulated rate. "rom the 7<o.e caustic solution tank in kerosene )ero unit. transfer enough material into pre!ash %essel H7 to hold sufficient le%el. Line up lean +9( from sulfur 5eco%ery 1nit to (mine surge drum 4E-H7. 9ntry of (mine in to H7 is controlled by 4E-L#-48 to maintain a le%el in the %essel. &he drum is maintained under pressure by blanketing !ith s!eet fuel gas a%ailable from fuel gas amine absorption unit. &he pressure controller 4E-P:#-D7 is a split range controller !ith 4 control %al%es one on fuel gas line and one on the flare line. 9stablish !orking le%el in amine scrubber c7, using 4E-P-4(0. and 4E-"5#-C. 9stablish +9( circulation putting into commission the le%el controller at bottom of the column to control the rich amine solution returning for regeneration in the sulfur reco%ery unit. (++:&:/> /" )95/M #(&(LKS&, A. S.
- 57 -

Ahile commissioning a fresh unit. there is no need to add catalyst in the beginning. Ae can add catalyst only !hen the circulating caustic becomes partly spent after absorption of )ercaptans from the LPG. .ut !e !ill describe the steps for adding the catalyst here. #alculate the appro imate -uantity amount of caustic circulating from regeneration to e tractor 4E-#-4 and back. &his !ill be e-ual to 76 to 78 'L. &he rate of addition of catalyst is appro imately a bottle for e%ery E ) D of circulating caustic. Prepare slurry of catalyst in caustic taken in a bucket. &hen transfer the slurry to the make-up pot. )i the slurry thoroughly in the pot by using (ir sparger pro%ided. &ransfer the solution under air pressure in to the circulating caustic. :t is desirable to add the total catalyst in small lots of 7 to 4 bottles at a time to ensure uniform distribution o%er the entire circulating caustic. Same principle for catalyst addition !ill be follo!ed !hene%er part of the caustic is replaced !ith "resh caustic to ensure minimum catalyst presence and acti%ity in the caustic. START-UP PROCEDURE

(fter the pre-commissioning acti%ities ha%e been completed the unit !ill be commissioned as per standard procedure noted belo!, #harge circulating caustic solution to top of e tractor column #4 after establishing a !orking le%el in disulphide separator HE in cracked LPG )ero 1nit. Ahen normal le%el of caustic is obtained in #4. commission the bottom le%el controller to regulate rich caustic flo! back to disulphide separator HE. #harge lean amine in flo! control to the amine scrubber #7. )aintain le%el at the bottom of #7 by commissioning the le%el controller regulating the rich amine flo! to regenerator section in S51. >/5)(L S&(5&-1P P5/#9+159 (t this stage all the chemicals are charged to the unit and the unit ready for taking in hydrocarbon. Line up cracked LPG flo! from battery limit to (mine scrubber -8 #austic pre!ash 2bottom t!o distributors3 -8 9 tractor-8 #austic settler -8 .ack pressure controller. #ommission the controller and set it at 7C kg0cm 4. /pen battery limit %al%e and direct LPG flo! to (mine scrubber. .e prepared to dra! more +9( from (mine regeneration unit as the (mine scrubber trays are being !ashed !ith (mine. Set the (mine flo! "5#.
- 58 -

"ill the scrubber, pre!ash and e tractor %essels !ith LPG, (s e tractor is being filled, caustic solution le%el in the regeneration section may be made to fill up the circulating caustic in%entory. )ake sure there is al!ays some caustic le%el in the e tractor. LPG should ne%er be allo!ed to enter regeneration section. /nce the unit is filled !ith LPG and is at the operating pressure 2of to 44 kg0cm4 at the inlet of the unit3, check LPG flo! rate and %erify all the gauge glasses. #ommission steam to caustic heater to maintain the inlet temperature to o idiser at EC= #. Start air in@ection. #ommission back pressure controller 4E-P#- 4E and set it at D.C kg0cm4. Send !aste air to %ent tank 4EH-C. #ommission o ygen analyser. /nce o ygen concentration in the %ent air is belo! 74G 2by %ol3, start fuel gas. Set "5J:-46 at a flo! rate such that o ygen content after dilution should fall belo! CG 2 by %ol 3. Send air0fuel gas mi ture to the highest disposal point in to the atmosphere. (s disulphide0caustic inter phase appears in the hori;ontal body of the disulphide separator, open disulphide oil disposal line to 4E-P-D. &he formation of disulphide oil !ill be %ery little and !ill be discharged to slop oil tank. &he pumping is e pected to be intermittent. )ake sure that some disulphide oil is seen in the sight glass of disulphide separator. +o not pump out caustic also. #heck the product after caustic settler for -uality. Ahen it is doctor negati%e, it can be routed to the regular storage bullets, kept ready for the purpose. #ommission odorant in@ection to the rundo!n LPG after caustic settler at the specified rate. #heck the odorant in@ection facility is ready in all respects beforehand. &hen start the :n@ection pump P-/4 and set the dosage as instructed. #heck fre-uently LPG for $4S after the pre!ash %essel H7 and replace cautic as necessary. #heck the acid oil content of the caustic solution once in a !eek. :f it is more then 8-74G then some caustic from H-7 !ill ha%e to be replaced. #heck the regenerated caustic being charged to the e tractor #4. &his !ill gi%e an idea of the efficient operation of disulphide separator . S#UTDOWN PROCEDURE ,

:nform all concerned of intention to shutdo!n the unit and proceed as follo!s , Shut off +9( charge pump to the scrubber #7. Shut off LPG charge pump to #7 immediately after this. Stop odorant in@ection pump P/ 4. Stop caustic circulation through the e tractor #4 from the disulphide separator HE. Stop caustic supply to pre-!ash %essel H7.
- 59 -

9mpty out caustic le%els from H7 #4 and H4 to spent caustic disposal or to the disulphide separator HE as instructed. 9mpty out +9( le%el in #7 to its regeneration section in S51. +epressure the %essels and columns slo!ly to the flare system, after isolation at unit limits. :solate the %essel and column by blinds and make them gas and chemicals free by steaming and !ater !ashing repeatedly, as per special instructions that !ill be issued at the time of shutdo!n. 'eep an upto date record of the blind list. 9ntry to the %essels has to be gi%en 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 gi%en. Proper %entilation inside the %essels must be ensured. Personnel entering the %essels must !ear proper protecti%e e-uipment as mentioned in the clearance permits. I. EMERGENCIES, POWER FAILURE

:n case of general po!er failure LPG supply to the unit !ill stop and the unit pumps running !ill be interrupted. +9( solution circulation also !ill stop. .lock of pressure controller at unit rundo!n line and hold pressure in the system. )onitor all le%els. Ahen po!er supply and LPG feed are restored, put the unit back into normal operation, follo!ing standard procedure. II. STEAM FAILURE

:n case of general steam failure, LPG supply to the unit !ill be affected and hence unit !ill ha%e to be shut do!n and kept under pressure till feed supply is resumed from "##. III. COOLING WATER FAILURE

"ailure of cooling !ater !ill affect the feed supply to the unit as !ell as the unit pumps. 1nit !ill ha%e to be shutdo!n and kept standby till !ater supply is restored. I$. INSTRUMENT AIR FAILURE

/n instrument air failure, all the control %al%es in the unit !ill close. :f "## is also affected by air failure. feed to the unit !ill be interrupted. #lose off the pressure
- 60 -

controller on LPG rundo!n line and maintain pressure in the system. )onitor all le%els till air supply is resumed to normal. 5e%ert back to normal operation. 7. 4. D. E. C. 6. OPERATING $ARIA"LES (mine concentration Lean +9( temperature +9( circulation rate LPG feed temperature :nlet pressure #austic pre!ash -4CG by !t. in !ater. -(s lo! as possible. -7< )D0$r. -DC to E<=#. -44 kg0cm4. -7<=.e 2#austic conc.3

#hange out the caustic at C<G spent or $4S break through. 7. 8. F. 7<. )ero causitic concentration #austic circulation rate 9 tractor inlet pressure -78 to 4<=.e.

-E )D0$r. -4< kg0cm4.

/ idi;er inlet temperature -EC to E8=#.

(ir in@ection to maintain 7.78 >)D0kg of )ercaptan Sulphur 2initially3 EC to 6< seconds, shake test. 8 to 74 %ol G of o ygen %ent gas. Lean )ero #austic #austic concentration -78 to 4<= .e. C< to 7<< !t ppm of >aS5 :f this figure is e ceeding dump out around 6 ) D of 4E-H-E caustic to 9&P , take fresh caustic into the system and add )ero 5eagent >o.4 as re-uired. LPG P59A(S$ LPG is passed through amine scrubber #7 and caustic pre!ash %essel H7 to remo%e all traces of hydrogen sulphide. &he +9( solution should be kept at the specified %alue of 4<G!t. &he amine circulation rate also should be at the design rate of 7< mD0hr. #austic concentration for pre!sh should be 7<=.e !hen it becomes spent. caustic must be replaced !ith fresh stock. LPG 9M&5(#&/5
- 61 -

)ercaptan e tractor #4 remo%es these undesirable components from LPG stream by intimate mi ing !ith a caustic solution containing )ero catalyst. &he caustic concentration for the circulation should be 4<=.e. &he catalyst concentration in the caustic should be 7<< ppm. )ero solution circulation rate should be E to C ) D0hr. /perating pressure !hich is maintained by the pressure controller on the rundo!n line should be about 78.< kg0cm4 at the e tractor #4. 5educing any of these %ariables e cepting the pressure !ill affect mercaptan e traction efficiency. &oo lo! an operating pressure fa%ours amine and caustic entrainment in LPG stream. I. TROU"LE S#OOTING MERCAPTAN EXTRACTION

)ercaptan 9 traction can be ad%ersely affected by one or a combination of the follo!ings , Poor )ercaptan o idation 2&his !ould be identified by a high )ercaptide #oncentration in the regenerated )ero #austic. &hat is *shake testI time too long3. &his is the most fre-uent cause of poor mercaptan e traction. ( dramatic increase in $ydrocarbon "eed and0or regenerated )ero temperature, for e ample, CC-6<=# %ersus EC=#. #austic

:ncrease )ercaptan content of the $ydrocarbon "eed, for e ample, higher mercaptan loading or higher molecular !eight mercaptan in the hydrocarbon feed. (ccumulation of non-regenerable acidic compounds or salts in the )ero #austic. &he most ob%ious effect is the consumption of caustic free alkalinity. &his problem can be identified by analysing the )ero #austic solution for G >a/$ as a strong base 21 P method 4<F3. &his %alue should al!ays be maintained abo%e 7< A&.G. Some of the undesirable compounds are $ 4S 2 as sodium sulfide3. carbon dio ide 2as sodium carbonate3, and sodium thiosulfate !hich is o idised sodium sulfide. Proper feed pre!ashing is essential in pre%enting the rapid contamination of )ero #austic !ith such compounds.#ontamination are purged by replacing a portion of the caustic in%entory in the system !ith fresh caustic. 2&he concentration should be chosen so as to keep the concentration in the )ero #austic bet!een 78 and 4C= .e3./nly plant /perating e perience can determine !hat is the ma imum allo!able concentration of each contaminant. 1psets in e tractor column hydraulics !hich are reflected as a marked reduction in e tractor tray efficiency, &his can be caused by partial %apori;ation of hydrocarbon in the e tractor, improperly stalled trays, e cessi%e hydrocarbon or caustic flo!s to the e tractor, etc. Partial hydrocarbon %apori;ation is the result of increased feed temperature or the inclusion of lighter compounds in the charge stock and0or lo!ering of e tractor operating pressure. (n upset in column hydraulics is e%idenced by e cessi%e caustic carryo%er !ith the e tracted hydrocarbon into the caustic settler. II. MEROX CAUSTIC REGENERATION
- 62 -

:mproper )ero #austic 5egeneration is caused by one or a combination of the follo!ing , (ir :n@ection is insufficient. :nsufficient air in@ection is -uickly ascertained by noting the o ygen content of the Hent Gas from the +isulfide Separator. ( %alue of less than 8 Hol. G / ygen !ould confirm that insufficient air is being in@ected. $o!e%er, this should be confirmed by a IShake &estI of the lean )ero #austic or by Laboratory (nalysis of the lean caustic for )ercaptide 2and Sulfide3. :mmediately check the (ir :n@ection System to %erify that air is flo!ing to the 5egeneration Section at the rate pre%iously established. :f there is reduced or no air flo!, re-establish proper air flo!. $o!e%er. if air in@ection is found to be at the pre%iously prescribed rate, then lack of sufficient regeneration air is probably due to , III. SULFIDE CONTAMINATION

( lead acetate paper check on the pre!ash hydrocarbon stream !ill determine if sulfide contamination is happening and determine its relati%e se%erity. :f the presence of $4S in the e tractor feed is confirmed, necessary steps must immediately be taken to re-establish proper hydrocarbon0+9( and pre!ash operation. :ncrease air in@ection in 7<G increments. :f there has been a sudden decrease in the Hent Gas / ygen concentration 2for e ample, 8 Hol. G to E Hol. G3. the cause is likely to be massi%e sulfide contamination. :t may be impossible to in@ect sufficient air to o idi;e all the sulfide on its initial pass through the regeneration system. :n this case air in@ection should be increased to its ma imum %alue. :t may be necessary for the sake of e pediency to permit the o ygen content to go higher than normal. )a imum air is limited to ma imum flo! meter and control %al%e capacity. &he disulfide separator pressure control %al%e should be monitored in this case. )a imum temperature at the o idi;er outlet should be 6<=#. &he inlet temperature should be C<-6<=# or as high as re-uired !ithout allo!ing the outlet temperature to e ceed 6<=#. Samples of the rich and lean )ero #austic should be sent to the Laboratory for )ercaptide and Sulfide (nalysis. Since the o idation of sulfide is an e othermic reaction substantial sulfide contamination is e%ident if temperature rise greater than D=# is noted across the o idi;er. :t may be necessary to note only increase in o idi;er temperature and pressure, but also begin purging the contaminated )ero #austic from the system !hen this is done, be sure to make up !ith fresh caustic of the correct concentration. Proper amount of catalyst should also be added. #ontinue taking these appropriate measures until the pre!ashed $ydrocarbon is free of $4S and the rich )ero #austic contains less than D<<< APP) Sodium &hiosulfate Periodic (nalysis of rich and lean caustic as !ell as check on the Hent Gas / ygen content !ill indicate !hen the sulfide has been completely o idi;ed to thiosulfate and proper )ercaptan / idation is re-established. (t this time reestablish normal o idi;er temperature and air in@ection conditions. Slo!ly add e tra mero catalyst to the system o%er a four hour period.
- 63 -

/n the other hand, should sulfide contamination be %erified but the source -uickly eliminated and the rich mero caustic analysis confirm lo! sulfide contamination. e. g. less than D<<< PP) >a 4S4/D immediately add some mero catalyst. say 7 litre of AS to the system. &he air in@ection rate may be increased at 7<G inter%als 2to maintain 2 8 -74 Hol. G o ygen in the Hent Gas3 and / idi;er inlet temperature increased so that the regeneration system !ill reco%er in fi%e to t!enty hours. I$. INCREASED SYSTEM MERCAPTAN LOAD

:f %arious checks outlined pre%iously indicate the absence of sulfide contamination, insufficient regeneration air is due solely to increased hydrocarbon flo! and0or increased system mercaptan concentration resulting in increased feed mercaptan loading. :n any e%ent, !ith increased air in@ection and temperature, the regeneration system !ill reco%er rapidly. (dditional catalyst make up may be considered at this time. )ero #austic flo! to the e tractor and increased air in@ection should ha%e been increased proportionately !ith any increase in )ercaptan loading from increased hydrocarbon feed rate. $. MEROX Ca/a-)2/ CONCENTRATION IS INSUFFICIENT

:nsufficient )ero #atalyst in the o idi;er and caustic solution is confirmed by the lean )ero #austic )ercaptan concentration greater then 4<< APP) 2or the IShake &estI time of longer than F< sec3, !hen the Hent Gas / ygen content is greater than 7FG. &his may be further confirmed by noting the physical appearance of the lean caustic. Lack of catalyst !ill lea%e the caustic solution pale green or e%en relati%ely colorless. :f this situation e ists, add 7 bottle of )ero AS o%er an eight hour period. "re-uently the problem is not too little catalyst or increased catalyst consumption, but improper addition of mero catalyst. &o pre%ent any loss of catalyst 2usually at the disulfide0caustic interface in the disulfide separator3. ( special effort should be made to al!ays add make up catalyst slo!ly and to mi it !ell to obtain a more uniform catalyst distribution. (lso ne%er o%er-o idi;e the )ero #austic 2e%idenced by blue rather than green lean )ero #austic3. "or this decrease the disperisibility of the )ero #atalyst causing catalyst loss. $I. OXIDI3ER TEMPERATURE IS TOO LOW

&he normal recommendation for the LPG )ero 1nit is to maintain the / idi;er :nlet temperature at the minimum re-uired in the range of D8-EC=#. (bo%e EC=#, o%er o idation reactions can actually lead to acid generation causing further caustic neutrali;ation. $o!e%er this temperature may be increased to C<-6< o# in instances re-uiring sulfide o idation. $II. EMULSIFICATION AND CAUSTIC ENTRTAINMENT

)ero #atalyst #austic Solution does not increase the tendency of caustic solution to emulsify !ith $ydrocarbon. :t does increase the detergent or foaming properties of caustic. #onse-uently, dirt and scale in e-uipment !ill be dislodged by )ero #austic. Part of this dirt or scale may consist of iron sulfide. &herefore, e-uipment
- 64 -

!hich is ne! or long out of ser%ice should be thoroughly flushed and cleaned before being commissioned or it may be necessary to discard the first batch of caustic if it becomes subse-uently loaded !ith iron sulfide scale from improperly conditioned e-uipment. (lso, certain corrosion inhibitors or the acid treatment of the inhibitor, promote emulsion problems &he inhibitor is picked up by the )ero #austic from the LPG being treated. &he presence of inhibitor or e cessi%e concentrations of inhibitor can normally be traced to improper inhibitor in@ection and thus !ith proper additi%e control, the problem can be eliminated. $III. INADEQUATE DISULFIDE SEPARATION

Poor disulfide separation from the lean )ero caustic in the disulfide separator can be caused by surfactant materials, !hich keep the disulfide suspended in the caustic. +isulfides in the )ero #austic can be analy;ed by 1/P )ethod DFD. &he presence of surfactants in the lean )ero #austic can be determined by a surface tension test comparison bet!een plant and fresh )ero #austic. Plant and "resh )ero #austic are each shaken !ith e-ual %olume of isooctane. &he time re-uired for the hydrocarbon-caustic phase to separate completely is noted in each case. Significant difference in surface tension and settling time is indicati%e of the presence of surfactant in the caustic. &he settling time for the plant )ero #austic !ill be significantly longer if surfacants are present. :f the )ero #austic is not sufficiently regenerated !hen lea%ing the o idi;er, some further mercaptan to disulfide may occur in the settling compartment of the disulfide separator do!n stream of the coalescing section. (ny disulfide formed there !ill not ha%e been coalesced into sufficiently large droplets to gra%ity separate from the caustic and !ill remain suspended. #omparison of the )ercaptan content of the #austic sampled at the o idi;er outlet and disulfide separator caustic outlet !ill indicate the )ercaptan are o idi;ing to disulfides in the disulfide separator settling compartment. &his is usually caused by insufficient mero catalyst. or mi ing. Slo!ly add e tra )ero #atalyst and take steps to keep the )ero #atalyst suspended !ill eliminate this problem. :f insufficient separation is suspected, a Laboratory #oalescing &est can be conducted to check if dislfide separation could be impro%ed. :nsufficient separation is likely to be caused , :mproper installation of coalescing partition so that anthracite coal has migrated. :mproper installation of anthracite coal, or >o anthracite coal at all. (t the earliest opportunity the %essel should be opened and the situation %erified and corrected. Proper disulfide remo%al from the lean )ero #austic is imperati%e
- 65 -

if full benefit is to be recei%ed from the e traction operation. (ll of the disulfide cannot be gra%ity separated from the regenerated caustic. ( lo! re-entry sulfur concentration 2less than 7< PP) in the $ydrocarbon3 is considered ade-uate. IX. INADEQUATE PREWAS#ING

(side from the ob%ious cause associated !ith the break-through of acidic compounds due to e cessi%e -uantities of $ 4S or #/4 in the feed or Spent #austic, the only remaining cause for a problem is inade-uate contacting or mi ing in the pre!ash. &his is caused by insufficient hydrocarbon flo!. $ydrocarbon distribution into the batch caustic is insufficient to assure proper mi ing and contact. &his situation can only be corrected by plugging some distributor holes. &he number of holes to be plugged should be propertionate to the decrease in feed rate.

- 66 -

4. U-2& CRAC ED FCCG MEROX UNIT CAPACITY

#racked >aphtha )ero 1nit is designed to Process D<<,<<< &0Kr.of cracked gasolene and Straight 5un gasoleneO the LS5 component being 6<,<<< &0Kr. &he 1nit Shall operate for DEC on stream days in a year. 2i3 2ii3 2iii3 2i%3 2%3 2%i3 FEED SPECIFICATIONS .oiling range &.P oc Sp. Gra%ity at 7C.6=# &otal Sulphur !t. ppm. )ercaptan Sulphur !t. ppm $4S !t. ppm 5HP , 'g0#m4 PRODUCT SPECIFICATIONS #C -F< <.67 7<< ma . 8C< I 7< I <.7 I

&he )ero treated gasolene shall meet the follo!ing specifications , 2a3 #opper strip corrosion 2D$rs.at C<=#3 2b3 )ercaptan*S* !t. ppm 2c3 / idation stability minutes C )a 1/P -76D -64 DF< min. (S&) + -C4C -CC 7 )a (S&) +-7D<-6C

TYPE OF CATALYST USED

#austic dispersible )ero 2catalyst AS supplied by 1ni%ersal /il Products #ompany, :llinois 1S(, is used in the s!eetening 5eactor 4CH4 of this unit. :nitial charge of catalyst about Dkg of acti%e ingredient of catalyst. Ahene%er caustic solution is replaced, catalyst make up is necessary. >ormally !e use 74) D of >a/$ of 8G concentration. &he catalyst make up is 7 kg. of acti%e ingredient for e%ery E 'L of caustic. Ahen the circulating caustic becomes more than C<G spent, the entire caustic should be discarded to 9ffluent &reatment Plant and fresh catalyst should be taken in as detailed abo%e, follo!ed by addition of fresh catalyst to the caustic. DETAILED DESCRIPTION OF P!ID

)ero treatment of S5> and "## gasolene consist of #austic pre!ash

- 67 -

Li-uid-li-uid s!eetening #austic settling Passing through sand filter #austic pre!ash is pro%ided on for straight 5un naphtha, as "## Gasolene after stripper and +ebutaniser contains little or no $ydrogen Sulphide. "or s!eetening proper a mi er type of 5eactor has been pro%ided. Post treatment consists of a caustic settler and sand filter. (nti-o idant in@ection facility is also pro%ided. Straight-run naptha stabilisation from distillation unit stabiliser is Icharged to the unit by feed pumps <4C P4 (B.. &he flo!-rate is controlled by <4C "5#-7. and is taken into caustic pre!ash %essel <4C H7 P7<< 6<<3. &here are three inlet no;;les and a stainless steel !ire mesh at the top as in other pre!ash %essels. #austic is to be changed out as indicated by its strength. "## gasolene from gas concentration section stabiliser bottom @oins straight run naptha at the outlet of caustic pre!ash %essel and the mi ture goes to the mero 5eactor. &he flo! of "## gasolene into mero is recorded by <4C "5 7E. &he combined flo! of naphtha and gasolene is recorded by <4C "5 E. #austic !ith suspended mero #atalyst >o.4 is added to combined hydrocarbon under <4C "5# 7< flo! control. (ir re-uired for o idation is added to the combined stream plus caustic through a special check %al%e <4C y 7 !hich ensures thorough mi ing of air and hydrocarbon. (ir flo! rate is controlled by <4C "5# C. &he reactor <4C H4 276<< 67<<3 is a li-uid-:i-uid s!eetener effected in a mi er %essel ha%ing perforated trays to achie%e intimate mi ing of hydrocarbon and caustic containing suspended mero catalyst in order to accomplish desired s!eetening reactions. 9ach tray has a total of 64 perforations distributed e%enly at four different radial distances. &he tray @oints are all fi ed !ith neoprene gasket to a%oid any leakage at @oints !hich !ould affect mi ing efficiency. &he mi ture of hydrocarbon, air and caustic containing catalyst rises up the mi er through the perforated plates and e its at the top of %essel and goes to caustic settler %essel <4C HD 24E<< F<<<3. &he mi ture enters the settler through a %ertical slotted pipe distributor. &he hydrocarbon lea%es from the top of settler to sand filter <4C HE 244<< E8<<3. &he caustic containing mero catalyst settling do!n at the bottom of settler is !ithdra!n through a perforated riser pipe ha%ing C< >os. 708I holes placed circumferentially in a spiral fashion. &he riser pipe ensures !ithdra!al of clear caustic from the settler for circulating back to feed. &he settler caustic is pumped by pump <4C P7 (B. and circulated under flo! control <4C "5# 7<. "or addition of catalyst into circulating caustic stream, !hen necessary catalyst addition may be done through the pot <4CHC 2EC< F<<3 by pushing the catalyst solution by air pressure. &he hydrocarbon enters the top of sand filter through a distributor pipe assembly !ith holes drilled to a specified pattern. &he sand packing is pro%ided in the top half portion of %essel and supported at the le%el. $ydrocarbon filtering out of the sand bed is picked up from a high enough le%el to ensure clear hydrocarbon !ithdra!al. &he treated product is sent to storage after maintaining the necessary
- 68 -

back pressure in the unit by <4C P:# 74. :n@ection of 1/P >o.C antio idant !ith or !ithout copper deacti%ator is done by do;ing pumps 24DP-D(0.0#0+3 located in unit <4D. ( slip-stream of run-do!n product acts as a carrier for inhibitor discharging from the do;ing pump. Sand filter is pro%ided !ith a bypass. 9 cess unreacted air accumulating on top of sand filter can be %ented from the floor le%el itself by the e tended %ent line. "acility also e ists for back !ashing the sand-bed, if re-uired. &he treated product from the unit is a component of motor gasolene pool. >/&9, LS5 gasolene is no! not processed in 4C unit. 4CH7 is being used as knock out pot for sponge gas from 4<-#-4 to 4<-#-6. 4C-P-4(0. ha%e been remo%ed to other ser%ices and gasolene inlet and outlet lines ha%e been blinded. I. PRE-COMMISSIONING OPERATIONS C#EC ING COMPLETION OF CONSTRUCTION WOR ( INSPECTION AND "OXING UP OF EQUIPMENTS.

&he follo!ing preliminary operations !ill ha%e to be carried out to ensure a successful start-up of the unit , #heck that all mechanical !ork of construction ha%e been completed. (ll e-uipments and pipelines must be inspected and tested hydraulically at stipulated pressure depending on design conditions. &hey are to be bo ed up only after internal inspection for proper fittings and cleanliness. "inally, all unit e-uipments and lines are to be signed off as complete in all respects in the Production +eptt. check lists made for the purpose. )ake a final blind list indicating !hich should be in position and taken out before starting gas purging operations. 9nsure that all blinds ha%e been installed at the proper sides of %al%es and signed off in the list. #heck and ensure the a%ailability of "ire-fighting and safety e-uipment in the unit area in good !orking condition. 9nsure all utility systems and flare release header is in ser%ice and ready for use. #heck that free mo%ements inside the unit area are not obstructed by scaffoldings, construction debris, tools etc. Get them cleared a!ay from the unit area. :solate the unit from other plants and storage tanks at the unit limits !ith block %al%es, for carrying out flushing and purging operation. :solate to remo%e instrument orifice blocks for flushing purposes. II. WATER FLUS#ING OF T#E UNIT

Aater flushing of the entire unit has to be done !ith all pumps running on line so that all muck, scale and construction debris are !ashed out of all e-uipments and
- 69 -

lines. "or this purpose, the unit can be con%eniently di%ided into sections and indi%idual e-uipment !ise !ater flushing can be done, &emporary fire !ater hose connections are made on unit e-uipment or lines at suitable points and thorough flushing is done. Suitably !ire mesh strainers are to be installed on pump suction spools during the !ater flushing operation to protect the pumps from damages. &he pumps are to be run at least for 4E hours continuously to ensure their free and smooth functioning. +uring the !ater flushing operations, care should be taken to see that pump discharge %al%es are sufficiently throttled so as not to o%erload their motors. &he suction screens installed !ill ha%e to be opened up and cleared of all debris collected periodically after stopping the pumps, &his type of cleaning the screens !ill ha%e to be continued till they remain free of any muck continuously at least for 8 hours. /n completion of !ater flushing the unit e-uipments and lines satisfactorily, !e ha%e to pressure test entire system !ith steam. III. PRESSURE TEST ! PURGE EQUIPMENT AND LINES

:n order to check for leaks on e-uipment and lines after !ater flushing they are all tested !ith steam pressure of about C kg0cm 4 proceed as follo!s , .lock off caustic circulation pumps Pl ( B . !ith their suction, discharge %al%es. /pen !ide all %ents and drains in %essels Hl, H4, HD. :solate sand filter HE closing off its inlet and outlet %al%es. &he sand fi7ter is to be purged !ith gas and tested under gas pressure to a%oid caking of the sand bed. $ook up steam hoses to the steam out connections of the %essels Hl, H4 and HD and back up steam into the %essels and lines upto the unit limit block %al%e. (fter sufficient steam purging for about 7C minutes from all possible %ents and drains. #lose these points and pressure up the system to about C kg0cm4 !ith steam. #heck up the entire unit for leaks and get them attended. (fter successful completion of pressure test. continue !ith steam purging of the unit system till all air from e-uipment and lines ha%e been remo%ed. &he system is ready for taking in hydrocarbon !hen all air from the system has been displaced by steam. )aintain a positi%e pressure of steam till fuel gas is taken into the unit and it is pressured up !ith gas. "uel gas is slo!ly taken into the pre-!ash %essel H7 and then to mi er H4 and caustic settler HD. &he sand filter is also purged !ith gas first to displace all air and then pressured up to fuel gas system pressure. #atalyst addition pot HC must be isolated from the gas purging lines. +rain all steam condensate from lo! points and drains. Ahen gas smell comes out of the %ents of the %essels. steam can be completely shut off and system allo!ed to remain at <.C kg0cm4 pressure of fuel gas.

- 70 -

I$.

C#ARGING OF C#EMICALS AND CATALYST

.efore actual start-up of the unit, the treatment systems should be made ready to recei%e LS5 gasoline from (H1. Prepare system as belo!, Pump in 7<=.e caustic solution from storage tank in 'ero )ero establish !orking le%el in the pre!ash %essel H7. section and

#harge 7<o.e caustic solution into caustic settler HD from 'ero )ero section till sufficient le%el is obtained in the settler for circulating caustic through mi er H4. Prepare )ero catalyst slurry in catalyst addition pot HC. taking desired -uantity of catalyst in it !ith caustic and !ater to make the solution. 'eeping the %ent of HC open. (dd air through the air connection to the pot for proper mi ing of the slurry. &hen close the %ent and increase the pressure in the pot, to blo! the catalyst slurry into the system along !ith the caustic solution circulated through the mi er H4. #are should be taken not to blo! air into the system to a%oid e plosion. &he catalyst is blo!n into the system along!ith caustic circulating after introducing gasoline feed in the unit. #atalyst addition to the system has to be done in batches depending on the doctor test conducted on the treated gasoline. )ake ready the anti-o idant in@ection facility in %isbreaker >aphtha )ero section for dosage into the treated gasoline stream from the unit, before it is routed out to storage tanks. START-UP PROCEDURE

Ahen pre-commissioning operations in the unit ha%e been successfully completed and the entire system is under "uel gas pressure then $ydrocarbon can be taken directly into the unit. #onfirm straight run gasoline from (H1 is ready to be supplied for )ero treatment proceed further as follo!s, "ill up !ith straight run gasoline the unit %essel, %i;., pre!ash %essel H7, mi er H4, caustic settler HD and Sand filter HE, one by one !hich ha%e been kept under fuel gas presssure. Pressure up each %essel to about respecti%e operating pressure. Prepare )ero catalyst slurry in catalyst addition pot HE and keep it ready for blo!ing into the circulating caustic solution to the mi er H4. :nform 'erosene )ero section and charge 7< o.e caustic solution from there to the pre!ash %essel H7 and bring up normal operating caustic le%el. &ransfer caustic solution !ith the help of circulation pumps P7 (0. to the mi er H4. #ommission flo! controller to regulate the flo! to mi er. #ommission in@ection air system from kero )ero unit and start air in@ection to the mi er at specified rate on "5# control.

- 71 -

#ommission gasoline charge pumps and commence flo! !ith "5#-on line through the mi er H4 after pre!ashing stage in H7 5oute gasoline to storage passing through settler HD and sand filter HE, !ith the pressure in ser%ice. Start in@ecting the re-uired -uality of mero catalyst into the caustic stream going to the mi er H4, taking care not to blo! air into the system. .ring operating conditions to normal. Ahen cracked gasoline becomes a%ailable from G#1, charge it to the mi er H4. Start anti-o idant in@ection into the treated gasoline stream at the stipulated rate. &he abo%e procedure !as applicable !hen 4CH7 !as used as pre!ash %essel. >o! 4CH7 is being used as the additional 'nock /ut Pot for the sponge gases from 4<#4 to 4<#6. LS5 naphtha from (H1 is not processed in 4C 1nit. Ahen the precommisioning operations in the unit ha%e been completed and the unit is under fuel gas pressure, confirm #5 gasoline from "## is ready to be supplied for mero treatment proceed as follo!s , prepare mero catalyst slurry in the catalyst addition pot 4CHC and keep it ready for blo!ing into the circulating caustic solution to the mi er 4CH4. #harge 7<o.e caustic solution into 4CHD. Ahen cracked gasoline becomes a%ailable from G#1 charge to the mi er H4. &ransfer caustic solution !ith the help of 4CP7(0. to the mi er 4CH4 . commision controller 4C"5#7< to regulate flo!. #ommision air in@ection system and start air in@ection to the mi er at specified rate on 4C"5#C control. Start anti-o idant in@ection into the treated gasolene stream. S#UT DOWN PROCEDURE

.efore commencement of the shutdo!n, stop antio idant in@ection to the gasoline stream. &hen inform all concerned of intention to shutdo!n the plant and proceed as follo!s , Shut off air in@ection to mi er H4 and block off the %al%es. Stop cracked gasoline to mi er H4. #lose of pressure controller 24CP:#-743 on the gasoline rundo!n line an hold system pressure. . Pump out caustic from settler HD and mi er H4 to the disulphide separator or to spent caustic disposal system.
- 72 -

+isplace all gasoline from the %essels to the storage or slop tank !ith fire !ater. "inally drain all the !ater and hydrocarbons from the %essel taking care not to pull any %acuum in them. :solate %essels !ith blinds and steam them out thoroughly using the steam out connections pro%ided. +rain all condensate from lo! points. )aintain upto date record of blind list. Aater !ash the caustic %essels and sand filter and mi er !ith fire !ater repeatedly till they are free of chemicals and clear !ater flo! out from the drains freely. )ake sure that indi%idual e-uipment has been properly isolated by blinds and made gas and chemicals free, as per laid do!n procedure. #onduct a gas test before allo!ing entry inside a %essel. :nsist on protecti%e e-uipment being !orn by personnel entering in %essels in caustic and other chemicals ser%ice. I. EMERGENCIES POWER FAILURE

:f it is a general po!er failure, all the pumps in the unit !ill stop. "eed to the unit !ill also be interrupted. :n this case the plant has to be shutdo!n. "ollo! the steps gi%en belo!, Shut off air in@ection to mi er H4. #lose off the discharge %al%es of all pumps !hich ha%e stopped. Shut off pressure controller at unit limits and hold pressure in the system, till po!er supply is resumed. Start-up the unit, as per standard procedure as soon as po!er supply is restored. II. STEAM FAILURE

:f feed supply to the unit is interrupted due to general steam failureO unit !ill ha%e to shutdo!n and !ait for resumption of feed supply from (H10G#1. :f it is a local failure gasoline )ero treating section can continue to run, as long as possible. III. COOLING WATER FAILURE

&he unit !ill ha%e to be shutdo!n as pumps cooling !ater supply !ill be affected. as !ell as feed supply from (H10G#1. I$. INSTRUMENT AIR FAILURE

(ir failure !ill result in all the unit control %al%es operating in their fail safe positions. i. e., they !ill all close. :f feed supply is interrupted unit !ill ha%e to shutdo!n. /ther!ise unit can be operated !ith the control %al%es blocked off and
- 73 -

maintaining pressure and flo!s on bypass. Le%els in %essels !ill ha%e to be monitored till air supply is restored. $. UTILITY AIR FAILURE

:f the failure is only for a short duration unit operation can be continued normarly. :n the absence of o idising air in@ection, the mercaptan con%ersion efficiency drops off -uite rapidly. $ence, the product !ill ha%e to be slopped as soon as it is doctor positi%e. >ormal operations can be re%erted to !hen air in@ection is restarted and the product is on grade. OPERATING $ARIA"LES

:n the mi er H4, all hea%ier mercaptans are con%erted to disulphides. $ere, the operating %ariables are air in@ection rate, )ero catalyst concentration in caustic solution and circulating caustic strength. (ir in@ection rate should be Q 7.7C >)D0kg of sulphur con%erted. &oo much air !ill gi%e rise to continuous %enting from the sand filter HD and increases the fire ha;ard. )ero catalyst concentration should be 7<< ppm in the caustic solution #austic circulated should be 7<-4< deg. .e. /perating pressure of the )i er is about 8.E 'g0cm4, $ence, the pressure controller !ill ha%e to be set accordingly to gi%e the desired back pressure in the mi er. MODIFICATIONS

7. S5 >aphtha from (H1 is not treated in 4C unit as 4C unit capacity is being utilised !ith #5 gasoline. &o remo%e light mercaptans !hich can be remo%ed in pre!ash, modification !as done to route part of #5 gasoline to 4CH7. 4. "acility to use 4CH7 as additional knockout pot for sponge gas from 4<#4 to 4<#6 gasoline inlet and outlet kept blinded. D. >ame of the Scheme Scheme >o Scheme implemented on +escription of Scheme 5eason for modification Scheme for butane blend in )S )50PS0D<<04<<40E (prN<D Pro%ision of routing of butane rich streams from +epropaniser bottom in P51 to "##G line at the do!nstream of backpressure control %al%e in )ero . .utane stream addition is a %ery good media to increase octane. &his can be added to )S sub@ect to meeting the 5HP0HL: limit. &hus octane boost obtained after butane addition !ould be used to upgrade naphtha to )S.
- 74 -

/perating instructions

1" #uta!e rich stream from 18C1 $ottom is $le!ded i!to %-25 &'( to $oost the )cta!e of *+" ,his also helps i! up radatio! of additio!al -aphtha i!to *+" ,he $le!di! is do!e throu h a !ew co!trol valve 25-./C11090 provided at the dow!stream of %-25 #1C" 2" #uta!e $le!d i!to *+ also poses some ha2ards li3e additio! of more $uta!e i!to *+ ca! lead to *+ 4uality failure i! &51 6 57/ a!d ca! also lead to pote!tially da! erous situatio! i! *+ ta!3" 3" /!terloc3s provided i! $uta!e $le!d facility are 8 25-./C-1109 would close at 18C1 $ottom temp less tha! 92 (e C" 25-./C-1109 would close whe! 25-.&-4 9 .CC: flow to *ero; < falls $elow 10 m3'hr"

4" 25-./C-1109 would !ormally remai! o! ratio co!trol" &atio would $e set $etwee! 0"04 -0"07" ,his mea!s $uta!e flow would $e 0"04-0"07 times sum of &eformate a!d .CC: flow" But this facility is yet to be created" 5" =t prese!t 0 25-./C-1109 would remai! o! =uto a!d set poi!t has $ee! loc3ed at 6 *3'hr 9ma;<" ,his mea!s at all times whe! the co!trol valve is o! auto0 the $uta!e $le!di! ca! $e set at a flow e4ual to or less tha! 6 *3'hr"
6"

Please stop butane blend in the event of following 8

-o &eformate ru!dow! from C&% -o .CC% asoli!e ru!dow! 9/!terloc3 has $ee! provided o! this a!d $le!di! co!trol valve should automatically shutdow!< %pset co!ditio!s i! 1&%

7" #uta!e i! ,otal *+ pool 9&eformate>.CC% asoli!e>)?C% -aphtha>5#-< should $e limited to 3"5-4"0@w

- 75 -

5. SAFETY ! FIRE FIG#TING FACILITIES (ll the general safety rules and practices applicable to Petroleum 5efinery operations are to be follo!ed in )ero &reating Plants also. (dditionally some of the safety precautions to be taken in each case are presented belo!, I. C#EMICAL #ANDLING

#hemicals, (mine B #austic are used in this unit. 5ubber glo%es, aprons and face shields are supplied for any @ob in the chemical area of this unit and they should be used for any @ob here. (ny spillage of chemicals on the body can be !ashed off !ith copious amounts of !ater. ( safety sho!er is pro%ided in )ero 1nits for any chemical spillage-emergency on the body of any person. (ll safety e-uipment should be cleaned !ith !ater so that they can be safely re-used later on. CAUSTIC SODA' #austic solution, commonly called lye, used in )ero units is to be handled carefully !ith due precautions. Glo%es, Goggles and face shields must al!ays be used in the treating area for any @ob. Painful in@ury and possible blindness can result out of caustic splash into the eyes. ( safty sho!er is pro%ided in the treating area for !ashing the body immediately if an accident occur. :n case of caustic splash into the eyes, both the eyes must be thoroughly !ashed !ith plenty of !ater and the person should be sent for firstaid. (ll eye in@uries must be referred to proper medical attention after the first aid. Aorkmen should be made a!are of the fact that caustic does not gi%e immediate !arning of its presence on the skin by burning or irritDtion. .ut its presence on the skin can be recognised by its slippery, soapy feeling. ( doctor must be consulted immediately in case of a se%ere skin burn. :n %ie! of the ha;ards mentioned abo%e, !orkmen must !ear rubber glo%es and apron besides goggles and face shields !hen !orking in an area e posed to caustic. #austic is destructi%e to leather and it is ad%isable to !ear rubber foot!ear also !hile handling caustic. !hen caustic comes into contact !ith the skin, the area must immediately be !ashed !ith plenty of !ater. +epending upon the se%erity of e posure, !ashing !ith a 4G solution of acetic acid can be follo!ed. "ecilities for immediate !ashing !ith !ater like safety sho!er must be readily a%ailable in the caustic handling area. Pumps, %al%es and process e-uipment scheduled for maintenance must be flushed thoroughly !ith !ater prior to opening. )aintenance !orkmen must !ear all protecti%e e-uipment !hile doing @obs on e-uipment in caustic ser%ice. CATALYST ' )ero catalyst has no harmful effect on the skin. $o!e%er, !orkman should be ad%ised not to contaminate any part of their bodies !ith catalyst. Should any contact takes place, the catalyst must be carefully !ashed off the skin !ith copious
- 76 -

amount of soap and !ater until the blue colour is no longer seen. #atalyst should not be taken internally nor breathing of its dust permitted. DISULP#IDE +isulphides are high boiling oily organic li-uids ha%ing sp. gra%ity from <.FC to 7.<6. &hey ha%e an obno ious odour of onions. &hey may cause skin irritation and hence contact !ith skin should be a%oided. >o data is a%ailable about their dangerous properties. &hey should not be consumed. &hey are insoluble in !ater, but can be !ashed of the skin !ith !arm !ater and a good detergent. #lothes contaminated !ith disulphides must be remo%ed from the body. .reathing of their %apors is also not allo!ed. AMMONIA (mmonia gas leaks !ill be pungent and are easily detected by smell. &he cylinder should be immediately shut off. (mmonia gas is highly soluble in !ater and at lo! concentration of <.4 !t G, it does not present any critical safety problems. :f there is a spillage of (mmonia solution on the body, it should be !ashed, off !ith plenty of fresh !ater. "or storage and handling methanol all the safety precautions as applicable to gasoline should be follo!ed. II. FIRE FIG#TING FACILIITIES '

Portable +ry po!der e tinguishers and "oam e tinguishers are kept at %arious locations in the 1nits and can be used for all small fires.(ll the )ero 1nits are pro%ided !ith t!o parallel fire !ater mains one on east and another on !est side. &he normal pressure in these mains remains at 4kg0cm 4 and in case of fire, this pressure can be boosted upto 7< kg0cm 4. "ire !ater monitors !hich are pro%ided on the mains can di%ert the !ater @et to any angle !e re-uire and can be used for fire fighting+ry po!der e tinguishers, and foam e tinguishers of portable type are pro%ided in the unit at different locations for fighting small fires."or fighting bigger fires, fire !ater is a%ailable in the unit !hich is surrounded by fire !ater mains. &he normal pressure in the mains is about D to E kg0cm4.

- 77 -