Operating Manual

Ammonium Nitrate Plant

ABU Qir II

CHAPTER 1 FUNDAMENTALS
1. Physical properties of ammonium nitrate (AN , NH4NO3) 2. Advantage of ammonium nitrate 3. Disadvantage of ammonium nitrate 4. Additives to ammonium nitrate and its importance
4.1 Filler or Dolomite or The filling agent 4.2 Magnesium nitrate Mg(NO3)2 , the stabilizing agent 4.3 Granulating aid , surface active agent 4.4 Oil & amine coating

5. Row material used in the production of ammonium nitrate

5.1Ammonia liquid 5.2 Nitric acid 5.3 Filler , nature dolomite 5.4 Magnesium Oxide powder 5.5 Granulating aid 5.6 Coating agent

6. Introduction to process
6.1 Production of ammonium nitrate solution 6.2 Production of ammonium nitrate granules

General introduction
1. Physical properties of ammonium nitrate (AN,NH4NO3) :
Pure AN is a white crystalline salts . The Nitrogen content 35 % and oxygen content 60 % . The molecular weight is 80 . Produced from weak base and strong acid . Density at 20C , 1.725 gm / cm3 . Melting point 169.6C and decreased with increasing moisture content .

2. Advantage of ammonium nitrate :

The most famous nitrogenous fertilizers in the local and international areas . Having primary and secondary nutrients which keep it more useful for plants growth and nutrition . ( Nitrogen N2 & nitrate NO3 , Magnesium Mg & Calcium Ca ) High soluble in water . Used in the production of compound and mixed fertilizers NPK & UAN . Used as strong explosive agent in mines and in the manufacturing of explosives .

3. Disadvantage of ammonium nitrate :

Highly hygroscopic character which lead to caking and it absorb moisture at 60 % relative humidity . Must be more carefully during production and handling because of its explosion character due to chemical decomposition . Become corrosive after absorbing moisture .

4. Additives to ammonium nitrate and its importance :

Additives are added to ammonium nitrate to improve the physical , chemical and mechanical properties of AN to overcome its disadvantage .

4.1 Filler or Dolomite or The filling agent :

Mainly contain calcium carbonate and magnesium carbonate and magnesium carbonate CaCO3 , MgCO3 . Filler added to AN for decreasing nitrogen content in AN from 35% to 33.5% for decreasing the sensitivity of AN to detonation .

4.2 Magnesium nitrate Mg(NO3)2 , the stabilizing agent :

Magnesium nitrate solution with concentration about 30% Mg(NO3)2 . Mg(NO3)2 added to AN as stabilizing agent to AN against the thermal cycle to prevent AN granules from flaking or disintegration . It absorb the moisture from surface of granules and change it to crystalline water. Finally Mg(NO3)2 increases the hardness of granules .

4.3 Granulating aid , surface active agent :

It helps to collect and bind the small particles of AN inside granulator and real to the smallest surface area with granules (spherical shape) . It decreases dust emission inside granulator.

4.4 Oil & amine coating :

Mixture of oil & amine with special ratio . It cover and seal the granules from environment humidity to prevent AN granules from absorption of moisture and prevent caking formation . The ammonium nitrate produced after adding these additives has a good specification for using as fertilizer .

5. Row material used in the production of ammonium nitrate :

5.1Ammonia liquid :
The ammonia ( NH3 ) used in the production of AN is produced in ammonia plant at pressure 26 bar , temperature 25C and concentration 99 % .

5.2 Nitric acid :

The nitric acid ( HNO3 ) used in the production of AN is produced in the nitric acid plant U21 at pressure 6.5 bar , temperature 48C and concentration 60% .

5.3 Filler , nature dolomite :

Mainly calcium and magnesium carbonate , course sizes approx. 10 cm Composition , CaCO3 MgCO3 Iron as Fe2O3 Sodium a Na2O Potassium as K2O 54.1% 44.97% 0.01% 0.07% 0.01% Zinc as ZnO Silica as Sio2 Magnesium as MnO Moisture Chlorides max. 0.001 0.04 0.003 0.796 200 ppm

Size analysis after crushing and grinding , 99.5 % < 200 M & 90 % < 90 M

5.4 Magnesium Oxide powder :

It is a caustic calcination at moderate temperature of Magnesite mined from natural deposits presently exploited in Austria , Brazil , China , India , North Korea , Turkey , USA (Nevada ) & USSR . Composition , MgO content 85% abs , 90 % preferred Sio2 CaO 2% max. 2% max. H2O Chloride 3.5% max. 200ppmax.

Density (bulk ) Size

800 kg/m3

min. ( loose )

1200 kg/m3 max. (tamped ) 10 - 50 micron

5.5 Granulating aid :

It is a sulphonic acid solution , Composition , Specification : Density at ( 20C ) Viscosity ( 20C ) ( 50C ) ( 100C ) Flash point PH Solubility Crystallization temperature Color Storage temperature 1110 kg / m3 15 * 10-3 pas 20 -30 c stock 6 10 c stock > 150C 8 in water totally 0C white to yellow 15C - 50 C solids Water 35% 65%

5.6 Coating agent :

Alifatic primary amines , C12 C22 in mineral oil . Composition , Density Viscosity Flash point 30 % amines , 70 % Oil . 870 kg / m3 at 90C 896 kg / m3 at 50C 14 cp at 90C 26cp at 70C 150C , yellow color Form (amines) paste at room temperature .

6. Introduction to process :
6.1 Production of ammonium nitrate solution :
- UHDA vacuum neutralization method is used to produce AN solution . - The features of this process are , a-Simple and uncomplicated . b-Easy in operation and maintenance . c-Technically developed system . d-High degree of safety with regard to AN decomposition . e-AN produced with concentration from 91% to 93% without using heating steam . f-Low AN temperature during operation 150C 200C). g-Contaminated process condensate is used as process water for nitric acid plant . h-Small number of equipment used , - Reactor - Vapor separator scrubber. - Circulation pump. - AN produced by neutralization reaction between gaseous ammonia and liquid nitric acid (60% conc. ) , the heat of reaction is used to evaporate the water inlet (mainly from nitric acid ) by flash evaporator in vapor separator 31 C001 , the vapors resulted are cleaned in scrubber integrated in the vapor separator these vapors are condensed and stored in clean process condensate tank 31 D002 , but the contaminated condensate from scrubber 31 C00l is ( decomposition >

stored in process condensate tank 31 D001 which is transferred by pump to nitric acid plant . - AN produced at temperature about 135C with concentration from 91% to 93% and PH 6 - 7 stored in AN tank 31 T001 after increasing PH in neutralizer by adding ammonia gas . - Temperature of AN stored in 31 T001 is controlled by steam heating coils inside tank and AN circulated from tank to AN heater 31 E003 to prevent AN crystallization .

6.2 Production of ammonium nitrate granules :

- NSM or fluidized bed granulation process is used . - The features of this process are , a- The particle size enlargement by accretion which give a uniform and regular shape of granules . b- Start up and shutdown program in a short time . c- Produce granules with a low moisture content . d- Granules produced by this method have a good physical an mechanical properties . e- The slurry before granulation contain filler powder with AN concentrated solution . f- Magnesium nitrate solution and granulating aid are added to AN before granulation . g- The spraying inside granulator is carried out in the care of a fluidized layer by means of a large number of spray heads . - The way of granules formation inside granulator : The mode of granulation for fluidized bed granulator process is by accretion . Accretion means , growth by continuous evaporation and solidification of large number of minute drops of the solution on to the initial particle (seed or nucleus ) .
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- This mode of granulation (accretion) give fine and homogeneous structure to the granules and low residual of water content (moisture) . The granulator : It is empty vessel that contain a fluidized bed layer of AN granules and consists of : a-The lower casing . b-The perforated plant . c-The feed injection system. d-The upper casing . It consists of five chambers separated by baffles . The first three chambers are injection chambers where the slurry injection and sprayed in these chamber , chamber four for drying granules and chamber five for cooling , the fluidized layer has thickness of 1 meter , the fluidization air are fed and distributed by the perforated plate in all five chambers by fluidization air fan 32 K001 , and atomization air is fed by atomization air fan 32 K002 through tubes around solution injected pipes to atomize the slurry injected by nozzles , the granules moves along the granulator chambers from chamber 1- 2 - 3 their size increase by accretion ( note the seed material is introduced into the first chamber). - Fluidization air is heated by heater 32 E001A-E , chambers 1 , 2 , 3 about 100C & chamber 4 about 50C . - Atomization air is heated by heater 32 E002 to about 140C. - Slurry before injection to granulator mixed with magnesium nitrate , filler and granulating air and the concentration of AN in slurry approx. 97% . - Pressure inside granulator is vacuum , so the dust emission sucked by exhaust fan 32 K004 to scrubbing system which is recycled again to the system . - The solid circuit after granulator , Granules AN extracted by vibrating
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granulator extractor 32 H001 and through scalping screen 32 S001 to remove any lumps outlet from granulator , bucket elevator 32 H002 to screening section by screen feeder 32 H007 A/B , the granules screened by vibrating screen 32 S004 A/B which classified granules into three fractions (oversize , undersize , on-size ) oversize a undersize recycled again to granulator by recycled belt 32 H004 ( oversize crushed throw crusher 32 S006 before fed to granulator ) , on-size is sent to cooling section , the cooling section is tow stage , first cooler 32 E003 fluidized bed cooler decrease temperature of granules from 115C to 55C by using ambient air which is heated by heater 32 E004 to about 35C , the second and final cooling by final cooler fluidized bed cooler 32 E007 to decrease temperature of produced granules from 55C to 40C which is the storage temperature to bagging unit , the air used in final cooler is ambient air and humidity is removed from it by ammonia chiller 32 E008 and D009 moisture separation and air heated by steam heater 32 E009 then air fed to final cooler by final cooler fan 32 K007 . - Finally granules are lifted by bucket elevator 32 H003 to the coating drum 32 D011 where oil & amine sprayed by nozzle on surface of granules then transferred to bagging unit for storage or bagging . granules are elevated by

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CHAPTER 2 Description of process

I. Neutralization , ammonium nitrate solution
1.1 Ammonia evaporator 1.2 Neutralization reaction and reactor
1.2.1 The reactor 31R001 1.2.2 Vapor scrubber and condensation

1.3Ammonium nitrate storage

2. Granulation , ammonium nitrate granules

2.1 Production of magnesium nitrate 2.2 Slurry concentration section 2.3 granulator 32 R001 2.4 Solids circuit after granulator 2.5 Product cooling 2.6 Product coating 2.7 Air scrubbing

3. Steam uses : ( saturated steam ) 4. Preparation of filler before adding to ammonium nitrate and storage 5. Oil / Amine preparation Unit 34 6. Control parameters
6.1 Control parameters in the neutralization plant 6.2 Control parameters in the granulation plant

7. Critical points and problems

7.1 Ammonium nitrate solution unit ( U 31 ) : 7.2 Ammonium nitrate granulation unit ( U 32 ) : 8. Specification of AN solution produce
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9. Specification of AN granules I- Neutralization , ammonium nitrate solution :

1.1 Ammonia evaporation :
- Liquid ammonia fed from ammonia plant with temperature 25C and pressure 26 bar . - Ammonia evaporator 31E006 is used to evaporate ammonia liquid which is a horizontal heat exchanger ( shell and tube ) , integrated with droplet separator in the top . - Liquid ammonia enters the evaporator in the shell side and is evaporated by means of return cooling water flowing through the tubes , evaporation take place at varying evaporation temperature ( depends on water concentration and impurities inside the evaporation ) , and a pressure of about 6.5 bar . - The required evaporation pressure of gaseous ammonia is controlled by PV31207 and can be adjusted by changing of water flow through the tube and level of ammonia inside the evaporator . - Any droplets of ammonia liquid can be separated by droplet separator to be sure that the outlet ammonia from evaporator is completely gases . - In order to avoid accumulation of water in evaporator , part of NH 3 water mixture from 31E006 must be discharged into ammonia stripper 31E007 which return evaporated ammonia to system and remaining water with ammonia traces will be drained into the barrels .

1.2 Neutralization reaction and reactor :

- Equation of neutralization reaction NH3 (gas) + HNO3 (liq.) === NH4NO3 (liq.) + heat ( 145 KJ/mol ) 1 mol - Features of reaction a- Instantaneous reaction ( acid + base ) b- Exothermic reaction
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1 mol

1 mol

c- Occur at temperature about 140C to 150C d- Under pressure about 3 bar e- Acidic medium PH 2 -- 3 - From equation and chemical rules : a- The reaction proceed in the direction to produce ammonium nitrate when heat of reaction is drown . b- Number of moles inlet reaction is higher than number of moles outlet , it must happened under pressure . 1.2.1 The reactor 31R001 : Consists of three parts 1-Lower part : In the outlet of circulation pump 31P001 , nitric acid fed through distributers with ammonium nitrate circulated . 2-Middle part : Containing 43 vertical tubes , each tube has 3 inclined rows of small holes ( nozzles ) each row has 7 holes . 3-Upper part : Upon tubes , ammonium nitrate produced distributed before fed to vacuum separator . - Importance of pressure inside reactor : * Circulation pump of ammonium nitrate 31P001 generate the pressure inside reactor . * This pressure can be fixed and adjusted by the orifice in the outlet line of reactor and before vapor scrubber . * The boiling pressure of ammonium nitrate solution at 150C and concentration 93% is 1.15 bar abs. . * So , to avoid boiling of ammonium nitrate inside reactor the pressure applied inside reactor must be higher than boiling pressure of ammonium nitrate and must be stable , also to avoid bubbles formation inside reactor and vapor separator . - Temperature and heat inside reactor : * Heat of reaction formed used to evaporate amount of water inlet ( mainly
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from nitric acid ) . * Ammonium nitrate solution is concentrated by heat of reaction and flashing after orifice and the vapors generated 120C . * By heat of reaction and flashing , ammonium nitrate is concentrated to about 91% . - Controlling the temperature of reactor : * Circulation ammonium nitrate pump prevent any over heating inside the system . * Cooling by flashing in vapor separator ( decrease temperature of ammonium nitrate ) . * Using spraying condensate inside vapor separator . - PH inside the reactor : The reaction takes place in acidic medium from 2 to 3 PH * To avoid instability and oscillation of PH from acidic to alkaline medium which make it difficult to measure . * The reaction takes place clearly in acidic medium . * To avoid and pick up any free ammonia in ammonium nitrate solution . The tow reactant ( nitric acid & ammonia ) preheated before introducing the reactor , nitric acid (60%) is heated in nitric acid heater 31E002 to approx. 55C to 60C , this help to maintain ammonium nitrate solution concentration and save some of their reaction heat because vapors from the flash evaporator are used as heating medium , and to avoid unsteady reaction and measuring conditions caused due to liquid ammonia in ammonia gas stream , ammonia heater 31E001 is installed to dry the ammonia gas , after this heater ammonia gas has a temperature of approx. 55C to 65C , the heating medium is vapors from steam ejectors . After filling the circulation loop ( reactor R001+ vapor separator C001+
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are sucked in vapor

separator and temperature of ammonium nitrate decreased from 150C to

ammonium nitrate circulation pump P001) by ammonium nitrate solution , nitric acid supplied to reactor (bottom part) through nitric acid distributers has a temperature 60C and pressure 6.5 bar and passes inside reactor tubes ( 43 tube ) , and NH3 gas fed to restore (middle part ) and passes through holes in the tube (21 hole in each tube ) the NH3 gas dissolved in AN solution inside reactor and the instantaneous reaction between nitric acid and NH3 dissolved in AN takes place to from new AN solution inside the closed loop , AN solution introduces the vapor separator and by flashing vapors separated and AN concentration solution is drown from over flow line in vapor separator and is directed to neutralizer 31R002 to increase PH from 3 to 6.5 by injection ammonia gas in neutralizer and transferred directly to ammonium nitrate storage tank 31T001 . Supplying of ammonia gases and nitric acid liquid into the reactor 31R001 is ratio controlled and automatically performed by measuring and control instruments . 1.2.2 Vapor scrubbing and condensation : - The process vapor from bottom of vapor separator 31C001 contain contaminations of ammonium nitrate , nitric acid and ammonia , to avoid nitrogen losses , the vapors are cleaned in scrubber installed in the upper part of the separator 31C001 , the scrubber equipped with 4 trays and demister , so the over heated vapors generated from flash evaporation are saturated and cleaned during passing the trays , the operating pressure of 31C001 is approx. 0.33 bar abs. . - Temperature of vapors generated from C001 is approx. 71C , these vapors are used as heating medium in the nitric acid heater 31E002 , other part which is the main vapor stream is condensed in vapor condenser 31E005 by means of cooling water , condensate formed from 31E005 with condensate formed from 31E001 ( ammonia heater ) are collected in clean process condensate tank 31D002 , this

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condensate is fed by means of clean condensate pump 32P006 back to the top of the scrubber 31C001 , and removed from the bottom as contaminated process condensate , and contaminated condensate is collected in process condensate tank 31D001 with clean condensate from nitric acid heater 31E002 . The vapor in vapor separator 31C001 , vapor condenser 31E005 , and nitric acid heater 31E002 is maintained by exhausting the inert form 31E005 and 31E002 by steam ejectors ( 31A001 & 31A002) , the vacuum is controlled by sucking more or less ballast air into vapor vacuum line upstream of 31E005 . The bottom part of vacuum separator 31C001 has the overflow line of ammonium nitrate , where ammonium nitrate concentrated solution ( 93 % ) declined from overflow line to the neutralizer .

1.3Ammonium nitrate storage :

Ammonium nitrate solution is stored in tank 31T001 with concentration from 90 % to 93 % , temperature 135C and PH 6.5 , when storing ammonium nitrate solution for longer time the ammoniacal PH change to acidic by loss of ammonia , the original PH value of 5.5 to 6.0 for storing has to be readjusted automatically by bubbling in a controlled quantity of ammonia gas in to 31T001 , the storage tank has a heating steam coil ( walls & bottom ) , to prevent different layers of ammonium nitrate solution and crystallization on the walls , and to increase the temperature of ammonium nitrate solution in the tank , the content is circulated and heated via ammonium nitrate circulation heater 31E003 by ammonium nitrate heater pump 31P004 , by this heater the temperature of ammonium nitrate is controlled and maintained at approx. 135C .

2. Granulation , ammonium nitrate granules :

2.1 Production of magnesium nitrate :
- The main raw material to produce magnesium nitrate is magnesium oxide MgO which is stored in a big bin 32D007 ( max. 90 t) . - Magnesium nitrate is produced by direct reaction between MgO and nitric acid

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( 60 % ) in presence of ammonium nitrate solution ( 91 % ) in magnesium nitrate reaction vessel 32D008 , equipped with 3 impeller agitator . Equation of reaction , MgO + 2HNO3 ==== Mg(NO3)2 + H2O + H2 + heat ( 850 Kcal / kg MgO ) - Feature of reaction a- Exothermic reaction b- Proceed at temperature 90C c- At atmospheric pressure d- At low PH ( 0.9 ) e- Agitator for good mixing between MgO solid powder and nitric acid solution . f- Occur in presence of ammonium nitrate solution ( 91% ) to form eutectic mixture which lower the crystallization point of the mix to 55C . - Removing the reaction heat is carried out by means of condensate flowing through a coil of MgN solution cooler 32E005 , the main medium for cooling is condensate coil which is cooled by cooling water in 32E005 . - After feeding MgO powder , nitric acid and ammonium nitrate solution with special ratio controlled , and controlling PH of reaction by ratio of nitric acid , and temperature controlled by cooling condensate coil with automatic valves , magnesium nitrate produced with concentration about 31 % and temperature 90C and PH 0.9 , which is sucked from D008 by MgN pump 32P006 , that recycles some of it to the reaction tank 32 D008 and sends the remainder to the system .

2.2 Slurry concentration section :

- This section is used to remove water and concentrate the feed mixture slurry before granulation . - The feed mixture slurry contains : a- Ammonium nitrate solution ( concentration 91 % , temperature 135C )

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b- AN/MgN solution ( concentration 31%/31% , temperature 90C ) c- Weak solution of ammonium nitrate (concentration 60% , temperature 40C) d- Dolomite filler powder Concentration of this slurry is happened by vertical heat exchanger 32E010 by using steam ( 12 bar , 189C , saturated ) as heating medium , this heat exchanger integrated with vacuum separator 32 C002 . - The three streams of AN , MgN/AN and weak solution of AN mixed in one stream and fed directly to evaporator 32E010 , the temperature of solution after concentration is approx. 168C , the solution introduces in the tube side of 32E010 and 12 bar heated steam in the shell side which converted into condensate after heat transfer , all water vapor generated from concentration are sucked by evacuation in vapor separator 32C002 ( equipped in the top of vertical heat exchanger ) and the condensate recycled again to the system , the concentrated solution mixture is drown from vapor separator directed to mixing vessel 32D005 to be mixed with dolomite before fed to granulation section , the concentration of slurry after evaporation is approx. 97 % . - The mixing vessel 32D005 is heated by steam coil ( 12 bar steam ) to maintain the temperature of slurry in 32D005 at 168C to 170C , the slurry is drown from the mixing vessel and injected with the granulating aid ( by granulating aid metering pump 32P002 ) to granulator by variable speed granulator feed pump 32P001 .

2.3 Granulator 32 R001 :

- It is a fluidized bed type granulator consists of : a- Lower casing b- Upper casing c- The perforated plate d- The combined AN solution / air injection headers . - The lower casing supports the perforated plate and incases the injection system ,
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this casing is partitioned in five chambers pressurized by the fluidization air , the first three chambers house the injection system , the fourth chamber is empty and be heated and used for drying , the fifth is empty and only used for precooling . - The upper casing is made up by five chambers , the first three ones where AN slurry is injected and the tow last chambers where some granules cooling , drying is obtained . - The perforated plate , distributes fluidization air to fluidize the solids , it has very small holes with specific direction to move the granules from chamber one to chamber five . - The slurry and atomization air risers run vertically across the tow plates of the under casing . - The injection system is made up by the ammonium nitrate slurry spray heads and the atomization air nozzles , the slurry injected in the first three chambers , the injection chambers in the lower casing feature five straight ammonium nitrate slurry headers , each header bearing from 7 or 8 risers , spray nozzles top them and spray the slurry vertically upwards onto the seed particles , each injection chamber has 5 straight ammonium nitrate slurry header , ( 3 main headers , one in each chamber ) , and there is a circulation stream line of ammonium nitrate solution from 32P001 to mixing vessel 32D005 . * Fluidization air : - An ambient air delivered by fluidization air fan 32K001 and fed to the five chambers of granulator , the first four ducts to the chambers are equipped with heaters 32E001A/B/C/D , and chamber five has no heater ( cooling ) , and there is an air pre heater 32E001E working on hot steam condensate ( from 32E010 ) for the first four chambers . * Atomization air : - Is compressed by atomization air fan 32K002 to 0.4 bar gage and heated up to 140C by heater 32E002 before distribution in the undercasing . * Granulator scrubber :
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The dust generated inside granulator is about 5% of the plant out put , so the dust pre wetted dissolved and recycled again to the system in the form of weak solution AN which is stored in weak solution vessel 32 D004 , so the granulator scrubber used , it consists of a flooded elbow , venture element with slurry recirculation over granulator scrubber bottom pump 32P003 , cylindrical vessel with perforated plate flushed by 21 nozzles for spraying AN weak solution by pump 32 P005 , an irrigated mist eliminator . Air and dust from granulator 32R001 is exhausted at 125C , prewetted by 4 spray nozzles of very weak solution of AN , then passes through the venture element (flow velocity increased and decreased ) so AN dust dissolved and fell in liquid level of weak AN solution , and the remainder dust passes through perforated plate in the top of scrubber which has condensate with weak AN solution level and 21 spray nozzles , then the air is sucked by exhaust fan 32 K004 with a very small amount of dust ( 27 ppm ) to the environment .

2.4 Solids circuit after granulator :

- The granules of AN is discharged from granulator 32R001 at temperature 115C through vibrator 32H001 granulator extractor to scalping screen 32S001 and elevated by bucket elevator 32H002 to screening section through screen feeder 32H007AB. - The granules classified by vibrating screen 32 S004 A/B to 3 fraction , over size > 4 mm which is crushed by crusher 32S006 , under size < 2 mm , these 2 fractions are recycled again to the granulator by recycle belt 32 H004 to the first chamber of R001 to be the seed , the third fraction is one size or normal size from 2 to 4 mm which is the product .

2.5 Product cooling :

- There are 2 stages for cooling the product by fluidized bed cooler type which consists of : a-Lower casing . For introducing the fluidization air .
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b- Perforated plate. For distributing air and director . c-Upper casing For sucking the dust generated and reused again . a.The first fluidized bed cooler 32 E003 : The product from screening section down to first cooler at temperature about 110C and cooled in 32 E003 to 55C . - The ambient air is sucked by first fluidization air fan 32 K003 which is heated firstly by steam heater 32 E004 to about 35C to be sure that air is dry , then the air is distributed through perforated plate directed the air to move the granules and fluidize the granules to the outlet of cooler , the cooler end has a flap which control the level and residence time of granules inside cooler ( so we can control the temperature of granules outlet from cooler ) . - The small particles and dust from cooler is sucked by exhaust fan 32 K005 to send this dust to the cooler scrubber to be recycled again to the system . - The granules intermediate temperature in the discharge of cooler 32 E003 must remain within the 50C to 60C range, preferable at around 55 C , this is important to avoid promoting the occurrence of a metastable crystallographic characteristics . b.The final fluidized bed cooler 32 E007 : The 2 cooling stages are not immediately subsequent but are interrupted by a retention phase during which the granules are hold up for around 5 minutes in hold up bin D010 . - The AN granules are cooled in final cooler 32 E007 from 55C to 40 C which is the temperature required for storage and this temperature must remain above the crystallographic transition temperature ( 32C ) as thanks to the magnesium nitrate presence product stability is yet already achieved.
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transition

detrimental

to

the

product

physical

- To prevent moisture pick up the granules while in the cooler , the air relative humidity must be lower than 30% . - The fluidization air for final cooler is sucked by fan 32 K007 , the air passes through NH3 liquid chiller tube to separate the moisture content in the fluidized air ( the NH3 chiller 32 E008 , moisture separator D009 ), then the air is heated by steam heater 32 E009 , cooling for air by NH3 chiller is down to 6C and reheated to 25C by this way , to insure that air for final cooling has low moisture content and dry , this is all done in the suction of the air stream fan K007 , the discharge air stream fed to the lower casing of the cooler and passes through the perforated plate to be in a direct contact with granules and fluidized granules are cooled , the end of cooler has a flap to control the level of granules bed and the residence time of granules inside cooler . -Then the granules are taken up by bucket elevator 32H003 to the coating section .

2.6 Product coating :

- Finally the product is coated in rotary coating drum 32D011 with a liquid mixture of oil and amine metered with reciprocating oil / amine metering pump 34P003 and sprayed to the granules inside coating drum by spraying nozzles which give the umbrella shape with good distribution to the surface of the granules . - The product after coating transferred directly to the bagging unit for storage .

2.7 Air scrubbing :

- There are tow main location where dust is generated in the plant a- The granulator b- The fluidized bed coolers - Other sources for dust are ,

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a- MgO bin b- The crusher ( 32S006 ) c- The damping points on belts d- The elevator heads e- The screens -These sources of dust are connected to dedusting system carried through dedusting fan 32K006 , which sucked these sources of dust and discharge it to standard cylindrical scrubber 32C003 which are dissolved by condensate to form weak solution of ammonium nitrate which down to weak solution vessel 32D004 and used again in the system . a-Granulator emission : - This emission is the largest dust load , around 5 % of the total plant output . - Recycled again to the system by granulator scrubber 32C001 to weak solution vessel of AN 32D004 and to concentration section . b-Cooler emission : - This emission is about 1 % of the total plant output . - Recycled again to the system by cooler scrubber 32C003 to weak solution vessel of AN 32D004 and to concentration section .

3. Steam uses : ( saturated steam )

a- Steam 12 bar , temperature 189 C - For steam tracing for AN solution line - Heating fluidization air 32E001A/C , TV 32023/ 123 - Heating atomization air 32E002 , TV 32016 / 116 - Heating mixing vessel 32D005 , TV 32012 / 112 - Concentration section 32E010 , TV 32011 / 111 - Heating fluidization cooling air first cooler , TV 32042 / 142

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- Heating fluidization cooling air second cooler , TV 32044 / 144 - Heating air for filler mill 33S002 , TV 33001 - Steam ejectors 3201/02 A001 ( 3201/02 E006 ) b- Steam 7 bar , temperature 168 C - Service steam in unit 31 & 32 - Heating stripper of ammonia 32E014 - Steam for flushing of filters , pumps and headers - Steam tracing for ammonium nitrate lines - Heating of weak solution vessel 32D004 C- steam 4.5 bar , - Unit 34 for heating 34 D001 , 34 D002 - Tracing for magnesium nitrate lines

4. Preparation of filler before adding to ammonium nitrate and storage :

- Dolomite comes in bulk sizes approx. 10 cm and stored in a large open area , transferred via loader to feed hopper for filler 33 D001 . - Then elevated by bucket elevator 33 H003 ( through filler feeder vibrator 33H001 ) , then filler is fed to precrusher where the dolomite precruched and 98 % of output is smaller than 1 cm . - The capacity of precrusher 33 S001 is 5 t/h . - The crushed filler with size 1 cm is stored in filler bin 33 D002 . - Then the dolomite with size 1 cm is fed via feeder 33 H004 to the filler mill , where the filler is grinded from size 1 cm to powder , its capacity is also approx. 5 t/h the dolomite powder is separated by bag filters 33 F002 and pulsation air then stored in filler bin 32 D002 .

5. Oil / Amine preparation Unit 34 :

- Oil is stored in tank 34 T001 which is heated by condensate to maintain its temperature at 80C .
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- Amine is a solid material which comes in barrels and added in preparation tank 34 D001 with oil , dissolved , agitated and mixed , the oil / amine mixture has an amine concentration 20 % to 30 % oil / amine . - Then the batch is transferred to vessel tank 34 D002 which is heated by steam ( 4.5 bar ) to maintain its temperature at 70C .

6. Control parameters :
6.1 Control parameters in the neutralization plate :
1- Ammonia evaporator : Controlling parameter Controlling device Level of ammonia liquid inside LV 31501 evaporator 31E006 . Pressure of ammonia gas evaporator 31E006 . 2- Neutralization : from PV31207 , LV31501 , batches in stripper 31E007 , M/V of cooling water

Controlling parameter Controlling device Ratio between ammonia gas and liquid FV 31403 / 435 --- master , equipped nitric acid to reactor R001 . gas . Measure and control flow of liquid FV 31404 , 454 --- slave nitric acid . Measure and control PH value of AIC 31701 / 751 , it is connected as ammonium nitrate produced . PH of ammonium nitrate cascade to ratio controller NH3 : HNO3 inside AIC 31703 , by injection ammonia gas with TT 31015 / 017 and pressure Measure and control flow of ammonia compensation PT 31207 / 208

neutralizer 31R002 . Temperature of ammonium nitrate TIAHH 31011 / 111 solution at the exit of reactor 31R001 . TSAH 31012 / 112 3- Vapor scrubbing and condensation :

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Controlling parameter Controlling device Vacuum inside vapor separator Steam ejector , PV 31213 / 313 31C001. Flow of cleaned process condensate for FI 31407 / 457 31C001 . 4- Ammonium nitrate storage Controlling parameter Controlling device Ammonium nitrate solution TV 31 034 temperature . AIC 31 703 , AIC 31 711 PH of ammonium nitrate solution .

6.2 control parameters in the granulation plant :

1-Magnesium nitrate preparation loop : Controlling parameter Dosing weight of MgO powder . Controlling device Schenck control system 32 802 dosing screw 32H015 --- master Nitric acid quantity necessary to react FV 32 401 --- salve with MgO . Ammonium nitrate solution quantity FV 32 402 , FFIC 32 402 ( ratio ) ( 91 % ) corresponding to nitric acid flow Agitator 32 N002 Mixing inside reaction vessel 32D008 . FV 32 401 , FFIC 32 401 ( ratio ) PH of mixture inside reaction vessel 32D008 . by

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TV 32 001 A / B Temperature of reaction . LIC 32 501 , Gama Ray Level inside reaction vessel 32D008 . 2- Concentration section , mixing vessel and feeding pump : Controlling parameter Controlling device Flow of ammonium nitrate solution FV 32 403 / 453 --- master ( 91 % ) Flow of magnesium nitrate . FV 32 404 / 454 --- slave

Flow of ammonium nitrate weak FV 32 406 / 456 solution Level inside mixing vessel 32D005 . Dosing weight of filler . LIC 32 504 / 554 Schenck controlling system 32 811 / 861 by dosing screw 32 H016 Vacuum inside vapor separator 32C002 Steam ejector , PV 32 212 / 312 Temperature of ammonium nitrate TV 32 011 / 111 , TISHH 32 011 concentrated in 32C002 . Temperature of slurry inside mixing TV 32 012 / 112 vessel 32D005 . Pressure of granulator feed pump 32 PIC 32 213 / 312 P001 . 2. Granulator feed : a- Ammonium nitrate feed lines Controlling parameter
27

Controlling device

Bring the feed to pressure conditions Slurry filter for injection . b- Granulating aid Controlling parameter Amount of granulating Controlling device aid FFIX 32 419 / 469 , stroke of metering pump 32P002 corresponding to ammonium nitrate slurry fed to granulator . C- Atomization and fluidization air Controlling parameter Flow and pressure of atomization air . Temperature of atomization air . inside granulator ) . Temperature of fluidization air . 4- Product cooling : TV 32 023 / 123 Controlling device HIC 32 604/654 flap TV 32 016 / 116 Main recycle block valves Individual feed block valves

Pressure of fluidization air ( pressure PV 32 218 / 268 flap , HIC 32 6 flap

a-First fluidized bed cooler 32 E003 : Controlling parameter Controlling device Temperature of fluidized air inlet 32 TV 32 042 / 142 E003 . Temperature of product ( granules ) Exit flap in the end of cooler 32 E003 outlet cooler . Vacuum inside cooler 32 E003 . b-Hold up bin 32D10 : Controlling parameter Level of granules inside hold up bin Hold Controlling device up bin extractor 32 H008 TV 32 042 / 142 Manual flaps of exhaust fan 32 K005 and first fluidized cooler air fan 32 K003

controller ( vibrator ) C- Second fluidized bed cooler 32 E007 Controlling parameter Controlling device Temperature of fluidized air inlet 32 TV 32 044 / 144
28

E007 . Temperature of product . TV 32 044 / 144 Flap in the end of cooler Moisture content in air and in the final Ammonia chiller 32 E008 , moisture separator 32 D009 product .

7. Critical points and problems:

7.1 Ammonium nitrate solution unit ( U 31 ) :
1- Temperature of ammonium nitrate solution during operation and storage: - It is very important to follow and control the temperature of ammonium nitrate during operation and storage because of the high temperature leads to decomposition and explosion for ammonium nitrate and low temperature leads to crystallization for ammonium nitrate . - The operating temperature of ammonium nitrate during operation is approx. 148 C to 150 C , and during storage in tank 31 T001 is approx. 135 C . - The ammonium nitrate decomposition temperature is approx. 210 C which is far from operating temperature and the trip system in operation can save this point ( temperature alarm at 155 C & trip at 160 C and 170 C ) which stop injection ammonia and nitric acid . - The ammonium nitrate crystallization temperature is differ with different ammonium nitrate concentration , and there is a figure indicate this point , at 91 % ammonium nitrate concentration the crystallization point is approx. 99 C . - Note , the variation in the temperature is very quickly , so the controlling must be quickly . 2- False reading for transmitters of nitric acid and ammonia : - When the reading ( measuring ) of transmitter give false reading for nitric acid

29

or ammonia , this make a disturbance in the ratio controlled between ammonia and nitric acid and mainly affect on the temperature of reaction ( 31 011 / 111 ) and on the PH value ( 31 701 / 751 ) , if nitric acid increased , temperature and PH decreases , and if ammonia increased , temperature and PH increase and vacuum is slightly broken . - When these phenomena appear , the situation is controlled by changing the load of production ( decrease load ) to be sure and detect the false transmitter reading , then make complete shut down to check the transmitter by instrument group . 3- Blocking in vacuum line of PV 31213 / 313 : - In normal operation the opening of PV 31 213 / 313 is approx. from 50% to 70% , and vacuum is about 0.6 bar . - Sudden blocking in vacuum line ( from environment ) , so the vacuum inside vapor separator increased and affect the temperature of ammonium nitrate solution which decreased . - By quick check in location on PV 31 213 / 313 , the blocked line is discovered , and the situation is controlled by opening the manual valve ( slightly opening ) which sucked air from environment to adjust vacuum inside vapor separator and controlling temperature , then the maintenance group dismantle the blocked line , cleaned , erected again . 4- False reading for floating part of level glass for ammonia evaporator 31 E006 . - When the floating part of sight glass for ammonia evaporator 31 E006 suddenly raised and jammed at 100 % level on sight glass . - Trip for LV 31 501 happened ( closed completely , its trip at 90 % on 31 502 ) , and the level of ammonia liquid inside evaporator ( 31 E006 ) decreased , by quick check the problem is discovered and the situation is controlled by making bridge by instrument group to cancel this false signal ( trip 31 502 ) and readjust the floating part .
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- The same problem happened but the defect in the switch 31 502

( on sight

glass ) and the reading of sight glass is true , then the problem is solved by also making bridge on the signal 31 502 till changing the switch by instrument group .

7.2 Ammonium nitrate granulation unit ( U 32 ) :

* Magnesium nitrate loop : 1- The crystallization point or temperature of MgN mixture in reaction vessel 32D008 is about 55C , at this temperature the mixture start to from crystals which lead to problem "blocking in suction lines of pump and in the filter 32F001 , so the operating temperature is about 90C and can be controlled by TV 32001 A/B, also increasing temperature to about 100C make unsteady reaction and foaming . 2- Controlling PA is very important point , the PA at which proceed the reaction normally is 0.9 and can be controlled by amount of nitric acid fed and it's ratio "excess acid " . 3- Temperature indication is an important indication during operation on TIC 32001 which indicate if the reaction happened successfully or not , where the temperature decreased suddenly this mean that MgO powder fed is stuck or the chute of MgO blocked , and slightly decrease in the temperature may be means an excess acid , so sample must be taken to ensure the PH of the mixture concentration of MgN produced . * Granulation process : - Concentration section (32E010 + 32C002 ) 1- Temperature of concentrated slurry ( AN + MgN ) must be maintained at from 168C to 170C before injected to granulator , this temperature can be achieved by 12 bar steam from TV 32011/111 and the signal of this TV is taken from slurry (temperature) after concentration (in vapor separator) , so this temperature is controlled automatically.

31

2- Vacuum inside vapor separator 32C002 which is created by steam ejector (12 bar) and controlled automatically by PV 32213/313 and maintained at about -0.4 m bar , this is done to ensure that the vapor generated from concentration section is sucked and condensed to adjust temperature of slurry. 3- It is very important to save the tube of concentration section (vertical heat exchange ) 32E010from low PH and erosion by filler, so NH3 gas is injected before entering the slurry of AN/MgN to concentration section to increase PH of the slurry and in the final product and to save tube of E010 , and filler is fed to the slurry after concentration section . - Granulator feed pump 32 P001 : The important points to follow during operation 1-Temperature of pump TIAH 32066/67 which is about 165C 2-Steam of flushing must be completely closed. 3-Condensate seal and cool for packing of pump must be filled the conical . 4-If pump stopped , AN solution must be quickly drained from pump drains. - Granulator 32R001: By very good and high experience of engineers and technical for operating the granulator and dealing with problems , the shut down and start up for granulator takes place in a short time (shut down 2 hr &start up 1 hr) . 1-Vacuum inside granulator is created by PIC/HIC 218/611 , automatic controlled flap in the suction exhaust fan K004 , and venture element with 4 nozzle condensate from pump 32P003 . 2-Temperature inside granulator, is controlled by fluidization air heater 32E001 A/D/E by TV 32023/123 and is increased also by slurry temperature (170C) which is injected inside granulator , and the temperature of fluidization air must not permitted above 130C, and more over is detrimental for the granulation . 3-Granules size from granulator , can be slightly increased by increasing heat of fluidization air (TV023/123) and increasing ratio of MgN inlet to the
32

slurry before concentration section , this two actions can increase the granules size , and we are made a modified specification for screen analysis by this way . from 3.15 to 4 mm > 50% 3.15 to 2 mm >4.5 4.0 - 4.5 1.0 9.6 3.15- 4.0 50 2.0 - 3.15 38.8 < 2.0 0.6 2.0 - 4.5 98.4

4- Controlling the recycle ratio to from or to produce a uniform and homogeneous granules with a good spherical shape , by controlling the amount of recycle from crusher S006 which give the 3/4 of total recycle to granulator to be seed or nucleus for slurry injected . this amount can be controlled by vibrator in the shut of crusher S006 . 5- Continuous cleaning for screens S004A/B , continuous cleaning for screens every shift prevent increasing under size and helps to get a uniform shape for granules , 5-Granulator level , is controlled at about 50% and controlled by granulator extractor 32H001 (vibrator) and HIC flap value . * Cooling section for the product 1- Fluidization inside coolers E003/E007, must be good to ensure a direct contact between fluidization air for cooling and granules, T for first cooler E003 is about 55C (product temperature decreased from 110C to 55C) and T for final cooler E007 is 15C (product temperature decreases from 55C to 40C ) . 2- The granules from first cooler E003 must take a rest for about 5min in hold up bin D010, with a temperature 55C (from 50C to 60C )this is important to avoid promoting the occurrence of a metastable crystallographic transition detrimental to the product physical characteristics.
33

3- Thermal cycle for AN , and its crystalline states Transformation of the crystal states due to changing conditions ( temperature , pressure ) effect the physical properties of AN , the following crystalline states have been identified : System Temperature C State Volume change I >169.6 liquid 169.6 cubic + 2.1 II 125.2 tetragonal - 1.3 III 84.2 IV 32.3 V - 16.8 Tetragonal

rhomb rhomb ic + 3.6 ic - 2.9

- The phase transformation 4 to 3 at 32.3C is notorious for fertilizer producer , since the change in specific volume may cause fertilizer particles to degrade during storage and handling . This is especially important in subtropical countries ( like Egypt ) , where the stored AN can cycle back for the leading to disintegration of granules , which in turn leads to caking , excessive dust-formation and safety risks (detonation) . - So , as mentioned in additives part , magnesium nitrate added to AN to stabilize AN against the thermal cycle by raising the temperature at which crystalline states of AN change . - To test or detect the thermal stability of ammonium nitrate, this is happened by exposing AN granules to temperature change , 20 cycles between 15C and 45C and measuring the amount of increase of fines which must be maximum 1% ( below 1 mm ) . 4- Temperature of fluidized air fed to first cooler 32E003 must be about 36C because of the relative humidity of the air at cooler lower casing inlet must be lower than 45% to limit moisture absorption by the granules , & temperature of fluidized air fed to second cooler E007 must be about 25C and air relative

34

humidity must be lower than 30% (by NA3 chiller) , and the air water content is about 6g/kg dry air max . 5- Temperature of mixture oil & amine should be all the time below 70C to prevent the thermal degradation (never exceed 90C) .

8. Specification of AN solution produce :

Concentration Temperature PH Stored 90 % to 93 % 135C 6 to 7 at atmospheric pressure 33% 0.3% < 0.5 960 kg/m3 3.0 kp 67 40C 90 % > or = 2 - 4 92 % > or = 2 - 4.5 1%< 2

9. Specification of AN granules :
Total nitrogen content Free moisture Balk density Hardness PH Temperature to store Screen analysis

Section 3 Preparation of the plant for start-up

1. General
1.1 Inspection 1.1.1 Inspection of vessels and piping 1.2 Inspection of vessels and piping 1.2.1 Preparatory work 1.2.2 Electrical and instrumentation 1.2.3 Initial start-up of machinery 1.3 Checking of rotating equipment
35

1.3.1 Cleaning 1.3.2Mechanical cleaning 1.3.3 Flushing 1.3.4 Actions to be taken after cleaning

1.1 Inspection :
The aim is to check whether all plant equipment has been completely and correctly constructed as designed so that the plant as a whole can be commissioned in a safe and satisfactory way. All plant systems and sections have systematically and carefully to be checked according to following documentation: -Piping and instrument diagrams -Technical equipment specifications -equipment drawings -Isometric drawings and piping lists -Suppliers instructions
36

-Safety rules The checks should be started with the utility systems, i.e. steam, boiler feed water, cooling water, fire fighting water, instrument air, compressed air etc., since the utilities have to be available in the very beginning of commissioning and initial start up .

Material choice :
-Beware of copper parts in instrumentation, in pneumatic actuators, in oil systems, in miscellaneous accessory parts. -Carefully check material quality (SS) in all wet areas

Dimensional accuracy :
-Special attention for perforated plates of cooler: size, pattern and orientation of punched holes.

1.1.1 Inspection of vessels and piping :

Each vessel, drum, pipeline and duct from and to battery limit as well as within the plant between interconnecting lines and plant sections should be checked according to following guide lines : -Correct diameter and performance of pipeline. -Right connection at both ends of the line. -Correct position and execution of the branches. -Correct installation of valves and things. -Ensure that each safety valve installed has been correctly tagged and tested in the workshop on site to check the correct lift off and setting. -All safety valves must be correctly installed with a minimum of piping between the unit and the safety valve exhaust pipes free from siphons. -Correct flow direction of control valves, valves flowmeters, orifices, steam traps, check valves, strainers, etc. -Good accessibility to shut-off and control valves. -Correct and complete installation of instrument nozzles, sampling points,

37

etc. and its good accessibility. -Location of fixed points of pipes with good ability to expand at operating temperature. -Correct fixing of pipes and checking for none vibration. -Right materials for stuffing boxes at valves. The material of all valve stuffing boxes coming into contact with ammonium nitrate and/or nitric acid should especially be checked against specifications whether the correct materials have been provided. The packing must not be made from or contain any oxidizable (combustible) matter, nor must they be impregnated by such substances. -Necessary draining facilities complete and correctly installed at lowest points. -Necessary vent facilities complete and correctly installed at highest points especially of liquid systems. -Check all restriction orifices after its final installation. Check whether each orifice plate is installed with the correct size in its correct place. The final installation of orifices is to be executed not prior to the performance of pressure and tightness tests. -Correct alignment and fixing of all equipment. -Correct installation of all sight glasses, reference vessels for level control, and other instruments directly connected to vessels, etc. Any line blinds which were installed during erection for the purpose of blowing out, flushing or pressure testing, should be listed and drawn in the check diagrams. The line blind tags itself should be conspicuously marked by color. Start-up strainers should be installed in the suction line of each pump. These strainers must periodically be cleaned during precommissioning and may be removed after the lines are completely clean.

1.2 Preparatory work:

38

Remarks: Most of the following activities are to be carried out during erection time. Reports on scope of works and the results are to be handed over to the commissioning staff. After completion of erection and inspection of the plant the next step is general cleaning and preparation for initial start up of the plant as follows: -A general cleaning of the whole plant inside and outside of the building must be performed with the utmost care and thoroughness. -Since the whole plant at this state is still in an unsettled and uncleared condition, during all precommissioning works special attention has to be paid to the strict observation of safety rules. -All debris, scaffolds, tools etc. are to be removed ; walkways , doors , escapes to be unobstructed. -Trenches to be covered, and the entire plant floors to be cleaned. -All pipelines and equipment must carefully by cleaned first from outside and then from inside and a11 foreign matters must thoroughly be removed. -All safety equipment such as safety showers, respirators, gas masks, eyewash station etc. have to be available, checked and put in a condition ready for use. -All operators should advisably be instructed in necessary first aid procedures. They must also be instructed about locations and the use of all safety equipment available in the plant. -All utilities should be made available at battery limits in quantity and quality as specified such as : Fire fighting water Potable water Boiler feed water Cooling water
39

Electric power Steam Steam condensate Instrument air Plant air -All blinds within the plant used for hydraulic tests and insulation from battery limit shall be removed. -All telephone connections for emergency cases as well as to all interconnected and surrounding plants must be checked. -All pumps to be provided with temporary strainers or all strainers already installed for mechanical tests of pumps to be checked and cleaned. Kind of strainers should be in accordance with manufacturer's instructions. -Make sure that all pumps and other equipment requiring lubrication are sufficiently supplied with lubricants as specified by manufacturers.

1.2.1 Electrical and instrumentation:

Check whether the electricity supply is connected correctly and meets the specified data. Close all switches in motor control center for electric motors and other electrical equipment and adjust bi-relays at correct values. Make sure the electrical power is continuously available in all substations and at all consumers. -Turn on all panel lights and controls.
- Check all motors, gauges, levels glasses, transmitters, analyzers etc. to

open all of its block valves and close all bypasses. -Check carefully the right position in view of flow direction of all control
40

valves, valves, steam traps, strainers, check valves, flow meters. -Check all control valves in the pipe systems. Make sure that its downstream block valves are open and upstream block valves and the bypass valves are closed. -Check instrument air system to be sure that all block valves are open and system pressure is as specified. -Check all light bulbs of the alarm annunciator. -Check the proper function at control system. -Check the interlocking system carefully in accordance with the "Description of alarm and interlocking system". -When the electric power supply is started, check each electric motor separated from the machines, for its proper rotating direction.

1.2.2 Initial start-up of machinery:

-Prior to performing initial test runs of machinery, carefully study the manufacturers instructions of the special equipment. These instructions are in any way predominant for the preparation and handling of the individual equipment. -Fill all bearings and nears with suitable oil or grease. The types and quantities of lubricants are specified in the Manufacturers Instructions. -Next, disconnect the couplings between the driving motors and driven machinery, and check the motors for correct sense of rotation. -When performing initial test runs on machinery, strictly observe the special instructions of the equipment of supplier. -Only after a thorough rinsing procedure of the interconnecting piping systems, pumps should be subject to test runs, but initially only individually. -According to experiences made, during initial test runs of the machines

41

slight disturbances may occur, e.g. running hot of bearings, etc. Stop and restart a machine in intervals, if a bearing gets too warm. The reason for this very often is an overfilling with grease. Restart only after cooling down. -After its initial test run all pumps should run with clean water for an as long time as possible to smoothing the bearings to be well prepared for the initial start-up of the whole plant. Check: Stating of ammeter Motor/pump frequency ( rpm ) Bearings for eventual sings of overheating Gland packing box for overheating The sealing system for correct function. -If any indication of malfunction is found e.g. the pump bearing, casing or packing box overheats or discharge pressure falls, shut down immediately and investigate cause of the trouble and try to eliminate the problem before restarting the pump.

1.2.3 Checking of rotating equipment:

Pumps:
Each pump of the plant, even stand-by pumps, have to be checked individually according to following guide lines: -Ensure - if installed - that mechanical seals of pumps are o.k. and correctly installed in the specified material according to manufacturers specification. The mechanical seal must be absolutely clean and free of all foreign substances which could destroy it or lead to a bad function. -Check especially all pump stuffing boxes in AN-service whether they really do not contain combustible packing materials such as graphite or any other oxidizable substances.

42

-Check very carefully - if installed - the sealing and flushing water system at pumps for its completeness and correct installation. Test each system for its correct function under operating conditions prior to the initial startup of the pumps. -Check all installed restriction orifices in minimum flow lines and check their right tag numbers i.e. their correct sizes. -Install strainers and check filters for correct size and type of cartridge according to specification.

Blowers , Fans:
-Carefully check the inlet and outlet ducts and clean the ducts from all solid impurities. Pieces of wood, concrete or metal can be sucked in the blower and destroy the rotor. -Check impeller in balance. -Check vibrations of the drive and equipment during the test-run. -Control the temperature of bearings. -Check hydraulic beg of drains. -Check moving dampers (vanes)

Dosing Pumps:
Check according the following guidelines: -All pipes and vessels connected with the pipe are cleaned. -The stroke of all dosing pump is put on 0 mm. -Check the rotating direction of drive. -Check the lubrication of bearings. -fill the pump with the medium before start-up if the suction line has big H. -Open valves in the suction and discharge line.

43

Gears:
All preparation and start-up work should be done in accordance with the manufacturer instructions. -Check correct fastening. -Fill with seal or lubricates according to the instructions of manufacturer. -Check the function by test run without equipment. -Start with small load and increase the load step by step, if its possible. -Check the temperature of the gear by working under normal load. Oil temperatures up to 80 - 100 C are acceptable.

Belt drives:
In order to safeguard a perfect operation of the V-belt drives, it is imperative that the following directions should be strictly observed on assemblage: -The grooves of the two V-belt disks must be in strict alignment and free from arris, rust and dirt, before the V-belts are put on. -The driving and the driven shaft should be precisely parallel to each other in every direction. -Before putting on the V-belts, the distance of the shafts should be diminished as far as possible. No force nor mounting iron shall be applied, when putting on the belts. This should be done by hand in placing first of all each belt around the small disk and then putting it on the taller disk. After that the V-belts are preloaded, until they are evenly taut. -When the belts have been put on, the drive is to be set going and the machine to allow to run idle for about 15 minutes, in order that the Vbelts adapt themselves well to the grooves and deliver their initial tension. -Then the drive is to be shut down again, and on coasting the preload of 0,3 % of the belt length is to be set. -Especially in the first weeks after putting into service, care should be
44

taken that a possible elongation of the V-belt is compensated again by increasing the tension. It is also advisable to supervise from time to time the orderly belt tension, as possible slide-slipping might prematurely destroy the V-belts. -As normal V-belts are not resistant to oils, fats and chemicals, they must be protected from these materials. Should this not be feasible, we would recommend to use V-belt of conditionally airtight construction. -V-belts already shrunk up during operation must not run together in one set with new V-belts. If a few V-belts of multiple grooved V-belt drives should prematurely become unusable, a complete set of new belts is to be put on. As soon as these have shrunk up, they can be put together to sets with old, still usable V-belts.

Rotating Drums:
The drive system consists of the electric motor, reduction gear and girth gear pinion. The reduction gear may consist of a spur gear, bevel and spur gear, or planetary gear. V-belt drives, elastic couplings and starting clutches serve as a connection between motor and gear; gear and pinion shaft are connected by elastic couplings. The arrangement of the drive parts can be seen from a flow sheet attached to the operation instructions of manufacturer like mounting instructions and maintenance instructions of foreign parts. The drive pinion is wedged up on a shaft, carried in self-aligning roller bearings arranged in tandem. With an exception of the electric motor all parts are fitted on a basic frame in steel plate structure that has been machined at the contact areas of the drive parts. Previous to the first commissioning the gear has to be filled with the specified oil quantity. The bearings shall be supplied including grease filling and hence
45

ready for operation. The tension of the individual V-belt drives has to be checked. After some days of operation, however, the V-belt drive has to be tensioned again. The following rule of thumb may be applied : The end of the belt may be pressed in manually only by the profile height. During the mechanic trial run the performance of pinion and girth gear has to be checked exactly. The 2 internally recessed pitches have to be tangent. For this purpose the drum has to be rotated manually. The 2 pitches shall contact slightly at the lowest position, however, an overlapping is not allowed. An exact adjustment is effected by pressing or pulling of the running rollers. For this purpose heavy drums have to be lifted by a lifting device. The performance of the 2 pitches has to be checked several times as the drum lowers with increasing wear of the running rollers. Deep washing teeth will cause a higher load and with this an increased wear. The contact reflection of the teeth has to be checked carefully. If the teeth are not supporting over the total width the pinion may be adjusted slightly. For the commissioning we would advise you to apply a grinding paste for rough caste teeth. Preparations for first test should be done by manufacturer's specialist.

Crushers:
Following the erection and anchoring of the machine as well as the electrical connection of the motors the trial run can be carried out. Before trial run the following should be considered: Rotational direction of the electro motors Tensioning of V-belts Control of all bolting Control of machine interior for-foreign matter Checking of fitted chutes etc. above the machine for foreign matter.
46

During the trial run the temperature of the roller Plummer block has to be controlled continuously (see special instruction). The gap between the two rolls which determines the final grain size has to measured before material is fed into the machine, and must be corrected after the initial test crushing. The gap setting is carried out by means of the so called loose roll, i.e. after loosening the bearing foot screw one of the two rolls can be moved by means of spindles arranged on the bearings console. This setting must be carried out when machine is stationary and controlled through hinged bearing wall. Every shifting of the loose roll as well as the opening of the bearing wall must only be carried out when rolls are stationary.

Screw Conveyors:
Prior to commissioning the following points have to be observed: -Inspection if the erection complies with the erection requirements. -Inspection if the screw shaft turns freely on the whole way and if there are any foreign bodies in the conveyor, e.g. tools, construction material etc. -Inspection of all bearing points and stuffing sleeves regarding proper installation and grease filling and if the gear housings are filled with oil up to the marked oil level according to the lubrication instructions. -Checking if the operating voltage complies with the voltage mentioned on the motor performance plate and if the motors and other drive aggregates turn correctly in the conveying direction. -The safety switches and equipments have to be checked. -Prior to commissioning with material the screw conveyors have to run approx. 8 hours without material. During this period the bearing should above all be often checked regarding noises and warming up. Excessive

47

warming up could be the result of misalignment, so that in any case adjustments have to be made.

Elevators:
Start up and trial running must not take place until all safety switches have been wired up. All safety guards must be in place and doors and inspection covers closed. Before commissioning the following checks have to be made : -Tensioning the chains or belt. -The correct sense of rotation of the drive motor and the inching drive geared motor. -Note when checking: temporary removal of holding pin of anti run back bearing. -Oil filling of gear, anti run back device and coupling. -Removal of all tools and erection equipment. -Dedusting equipment. It is advisable to run the bucket elevator empty for a number of days (1-2) and thereafter, when the elevator is running perfectly, with material. Note: Prior to initial test runs of machinery, carefully study the Manufacturers' Instructions of the special equipment. These instructions are in any way predominant for the correct preparation and handling of the individual equipment.

1.3 Cleaning :
Before raw materials are admitted into the plant or a part of the plant, all lines and processing equipment items must be cleaned.

Cleaning. Mechanical Flushing.

48

Liquids Gases. Water Solution Air Steam. After-flushing.

1.3.1 Mechanical cleaning :

Mechanical cleaning may be necessary to remove large impurities which cannot be driven out by simply flushing with water (tanks, processing equipment). With pipelines, especially carbon-steel lines (rust) and lines which normally carry gases, mechanical cleaning is preferred to flushing.

3.1.3.2 Flushing : Preparations :

(Refer also to attached sheet "PRESSURE AND LEAKAGE TESTING OF PIPELINES") Draw up flushing diagrams with reference to the P & I-diagrams. Normally, the utility lines are flushed first, because these are used in flushing the installation. Indicate on the flushing diagrams: -The location of all blanks and flanges -The water and air connections, and the pumps to which they are linked -The valves to be opened and valves to be closed - all orifice plates and non-return valves -The draining points providing the fastest drainage of the liquid.

Requisites for flushing: -Sufficient water -Sufficient air free of oil -Hoses with appropriate couplings.
49

-Conical filters and blanks Note: The conical filters must be about 20-mesh; they are used to protect pumps and compressors. Blanks as well as filters must be provided with lips or other markers projecting from the flanged joint so that they may easily be found again. Flushing with liquids: Note: Care should be taken that the temperature of the flushing liquid does not exceed the maximum operating temperature of the equipment concerned. Flushing with water: - Uncouple lines at control valves, flow meters and pumps - Remove all process filters , orifice plates and non-return valves If possible, the flow velocity of the flushing water should be relative high (about 4-mlsec). Where possible flush from high to low. Start with main lines and pump suction lines. If possible, flush in the direction away from processing equipment items; should this be impossible, uncouple lines at these items. Flush separately 'dead' sections, e. g. by-passes around control valves, Rota meters, pockets in lines. In case of water is used for flushing, the chlorine-content of the water may never exceed 5 ppm, since otherwise alloyed materials suffer substantial damage. When the circulation of flushing water with such a CI-content is stopped the water should immediately be drained and must not remain in the equipment. So, after an extensive preflushing when the equipment seems to be clean , water with max. 1 ppm CI-content must be used for final flushing.

50

In order to increase the available quantity of flushing fluid, upstream equipment may be used as reservoirs. Prior to this it should be checked however, whether the platform will stand the load when the respective equipment is filled up with water.

Pumps Clean thoroughly and prepare for operation. Processing equipment: Fill completely and drain as rapidly as possible; during drainage, take care that no under pressure can develop. Flushing with solution: If the lines and/or process equipment items are seriously fouled, it may be necessary to use solvents for flushing. If oils and greases must be removed, for instance, flushing should be done with an alkaline cleaner not containing NaOH or KOH. See also maintenance manual. It will be clear that the nature of the solution to be used depends on the nature of the impurities.

After-flushing: After the flushing described above, circuits are established and water is circulated through them by the process pump. Filters should be checked regularly and, if necessary, fresh water must be taken. After thorough flushing,

51

the equipment is drained and internally cleaned where necessary (e. g. tanks and other vessels). This after-flushing must be carried out as soon as possible after flushing of the installation. Flushing with gases Air : By means of an air stream remove impurities from those lines which cannot be flushed with water for mechanical or dimensional reasons (strength, very large diameter). The velocity of the (oil-free) air stream should be relative high (about 30 m/sec.). If this velocity cannot be reached, other procedures will have to be resorted to. It is possible, for instance, to pressurize the line with air to the maximum allowable pressure (use safety valve) and then to release the pressure suddenly.

Steam: In general, only steam and condensate lines are subjected to a steam flushing. Disconnect the steam ejectors and flush the steam lines to these ejectors thoroughly. Special attention should be paid to safety (the direction of blow-off) and to the prevention of accumulation of condensate (which may give rise to water hammer).

1.3.3 Actions to be taken after cleaning:

Remove all blanks used for flushing purposes.

52

Install process orifice plates, process filters and non-return valves. Connect all line at control valves, flow meters and pumps. Where possible, the conical filters used in flushing should be left in the process lines. Be sure they are installed in the proper position.

Section 4 Start-up of the plant

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1. Neutralization (Unit 31)

1.1 Start-up conditions 1.2 NH3 evaporation
1.2.1 Preliminary operations 1.2.2 NH3 evaporation start

1.3 Neutralization
1.3.1 Starting with AN solution 1.3.2 Starting with demineralized water

1.4 Vapor scrubbing and condensation

1.4.1 Preliminary operations 1.4.2 Vapor scrubbing and condensation start

1.5 Ammonium nitrate solution tank

1.5.1 Preliminary operations 1.5.2 Operating

2. Granulation (Unit 32, 33, 34)

2.1 Solid system loading
2.1.1 Preliminary opera-ions 2.1.2 Granulator loading

2.2 Magnesium nitrate system

2.2.1 Preliminary operations 2.2.2 Magnesium nitrate reaction

2.3 Concentration system

2.3.1 Preliminary operations 2.3.2 Concentration start

2.4 Slurry system

2.4.1 Preliminary operations 2.4.2 Filler addition

2.5 Granulating aid system

2.5.1 Preliminary operations 2.5.2 Granulating aid injection

2.6 Slurry injection start

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2.6.1 Ultimate granulator air system adjustment 2.6.2 Effective slurry injection

2.7 Solids flow 2.8 Material coating

2.8.1 Preliminary operations 2.8.2 Coating start-up

2.9 Lime grinding 2.10 End product output 3. Summary of Start up Steps

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1. Neutralization (Unit 31): 1.1 Start-up conditions:

Following points should be fulfilled before first start-up - Water run must have been executed. - All valves and control valves must be closed and all control equipment must be set on manual. - Cooling water to all cooler, and condensers as well as NH 3-evaporator must be on line. - Granulation plant must be ready for taking over the AN-melt before start-up of unit 31.

1.2 Ammonia evaporation: 1.2.1 Preliminary operations:

NH3 evaporation consist of NH3 evaporator 31E006 and NH3 stripper 31E007. Note: Protective equipment according chap 7 has to be used during ammonia handling. Before filling the NH3 -evaporator system with liquid ammonia, the system should be dried. If necessary, ventilate with air when the compressor set is running to remove any water in the piping system from tests. Drain also pockets in gas lines. For preparation of the ammonia system check the position of all valves. All block valves and control valves in the liquid ammonia line to be closed. All block valves of instruments, such as gauges, transmitters, alarms, instrument air to be opened, vent and drain valves to be closed. All block valves of feed lines of ammonia stripper 31 E007 to be closed. Heater of NH3-stripper 31 E007 to be completely drained. Block valves in the ammonia gas lines to be closed. Set blinds in lines in adequate position downstream block valves. (These blinds can be removed if

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NH3 system is found tight) Make sure that full cooling water flow is passing the ammonia evaporator 31E006. Blow out the ammonia evaporation system with nitrogen via Nitrogen utility connections. All block valves up- and downstream of level control valve LV 31501 must be closed. 1.2.2 Ammonia evaporation start: Open the valve at battery limit slowly and carefully. Check the first part of the pipe system far leakage step by step. Open the next valves slowly and carefully. Feed liquid ammonia into NH 3 -separator 32-F004 resp. NH 3 evaporator 31 E006 in intervals and check system for leaks. To detect minor leaks, use of SO 2 from bottles is recommended. If ammonia system ?s tight, continue filling-up the system to approx. 20 % level in ammonia separator 32 F004resp. evaporator 31 E006, set controller LIC32511resp. LIC31501 accordingly and check the function of the controller. The two gas lines coming from 31 E006 and 32 F004 combine upstream of NH 3 -heater 31E001. During this procedure check the pressure in the evaporator system. Check the NH 3 -strippers 31E007 resp. 32E014. - Block valve upstream of AN-separator 31-D005 remains closed! Open only immediately before start up and -set pressure controller PICAL 31207 on automatic. Note: During this procedure goggles must be worn and gas masks - must - be kept ready. Closing the block valves in the NH 3 -liquid line may cause damages in the pipe by expansion of the liquid lockeo. in . Attention has therefore to be paid to the fact that only the valve at
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the inlet of the plant is tightly shut. All other valves shall only be operated (closed) in case of requirement (maintenance). Remark: According to German regulations (UVV) the NH 3 -System must be blown off with nitrogen, i.e. oxygen must not be in the system when filling with liquid ammonia. Preparation and filling of ammonia evaporation system also should be performed strictly in accordance with the local regulation.

Operating Instruction of the NH3 -Strippers

Stripping of NH 3 -evaporator 31E006 resp. of air chiller 32E008 is performed to get rid of the water which is introduced with the liquid ammonia. Stripping is done batch wise. It must not be done when neutralization plant does not work. During work at the ammonia bearing apparatuses have your personal protection equipment available: goggles, gloves, gas mask. NH 3 -Stripper 31E007 The consequence of water having accumulated in the NH 3 -evaporator 31E006 is an increase of temperature TI 31002 to approx. 23C, and at the same time pressure control valve PICAL 31207 is open to more than 70 % . So stripping becomes necessary. - Check level LI31503, and temperature TI31003 in NH 3 -stripper. Both must be on the low side; heating steam closed. Pressure PI 31203 is the same as PICAL31207. - Open drain valve at NH,-evaporator 31E005 and fill NH 3 -stripper 31E007 slowly to approx. 60 % of the level. Do it slowly as otherwise level controller_LICAH31501 may be affected. Close valve again. - Open heating steam slowly and stepwise, watch boiling by level glass LI31503. No ~water hammer, no vibration may occur.
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- As soon as level is down, and temperature TI 31003 has reached approx. 135 C, stripping is finished. Stop heating steam feed to stripper, and drain the liquid rest into a barrel. This has to be sent to a save location. (See Bid Clarification U2.21) NH 3 Stripper 32E014 The consequence of water having accumulated in the air chiller 32E008 is an increase of the temperature of the chilled air TI32048 to approx. 8C. So Stripping becomes necessary. - Check level 32513, and temperature TI32056 in NH 3 -stripper. Both must be on the low side; heating steam closed. - Check pressure in NH 3 stripper; pressure PI32234 has to be the same as PI32233. If not, open valve in the gas balancing line 50-AL-32286 to NH 3 -separator 32F004. Open drain valve at NH 3 -separator 32F006 and fill _ NH 3 -stripper 32E014 slowly to approx. 90 % of the level. Do it slowly as otherwise level controller LICAH 32511 may be affected. Close valve again. - Close valve in gas balancing line. Open valves in connection line 50-AL-32288 to NH 3 -stripper 31E007. Open heating steam slowly and stepwise, watch boiling by PI32234 and by level glass LI 32513. No water hammer, no vibration my occur. The liquid is pressed into NH 3 -stripper 31E007 by boiling pressure. Pressure must not exceed 7 bar, otherwise stop heating, and search for the failure. - As soon as level is down, stripping is finished, stop heating steam feed to stripper, and close valve in connection line 50-AL-32288 to NH 3 stripper 31E007. - Open valve in gas balancing line 50-AL-32286 to NH 3 -separator 32F004.

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1.3 Neutralization:
There are two alternative possibilities for the initial start up of the plant: - Starting with AN solution - Starting with demineralized water. An initial start-up of the AN reaction system by means of AN solution made available in 31T001 is in any way the more preferable of these alternatives. An initial start-up of the AN reaction system with demineralized water is the more difficult one and it needs more time in comparison with startingup with AN solution. The latter alternative is therefore the less preferable one. Which of these two alternatives for initial start-up finally to be applied is a question only to be decided in connection with the respective facts present on jobsite. 1.3.1 Starting with AN solution: Preparation works for initial start up with AN solution are to be performed in following steps - Prepare AN-solution tank according to the description in 4.1.5 - Prepare vapor scrubbing and condensation according to the description in 4.1.4 - Preheat carefully immediately before filling with AN solution AN neutralization loop with interconnecting piping by injection of heating steam via relevant local flushing nozzles. Stop injection of steam when all equipment is satisfactorily heated up just before filling in of AN solution and drain completely the steam condensate at all draining valves on heated up equipment and close

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properly all drain valves again. Filling of the preheated plant equipment with AN solution is to be performed as follows: - Open AN start-up line 50-AN-31129 (after reheating with steam) and fill AN-solution to the neutralization loop via suction line of the AN circulation pump 31P001 - Check if pump 31P005 is running for having available seal and rinsing water for AN circulation pump 31 P001, as well as injection water for 31C001 - As soon as AN-solution overflow to 31R002, start AN circulation pump 31P001. By circulating the AN-solution, heat is introduced into the system by pump 31P001 - Close the start-up line 50-AN31129 after 31 R002 is overflowing to 31T001 and clean the line with steam - Operate 31 P004 on circulation through 31E003 - Check pH-value of AN-solution in tank 31T001 and adjust to PH= 5.5 Start vacuum pumps 31A001 and 31A002 and evacuate the neutralization slowly - Set pressure controller PV 31213/313 for the beginning to P= 0.6 bar A and place controller on "automatic" - Watch the temperature in neutralization loop for sufficient "t" to the crystallization point. "t" should never be lower than 5 K. - Put set point of NH 3 -gasflow _ controler and HN0 3 -flow controller to zero - Override the interlocking system - Start pH-value measuring ARCAHL 31701/751 of AN neutralization; set controller to pH = 2.5 but leave it still on "manual". When starting open at first demin. water and adjust a quantity of approx. 60 - 80 I/h. Then add such a quantity of AN solution that the resulting weak AN solution sample gets a temperature of approx. 50 - 60 C
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- Open gradually and alternately in very small steps first a bit the HNO 3 flow control valve and after that the NH flow control valve by "manual" operation of the relevant controllers and repeat this in small time intervals until the plant load has reached approx. 25 - 30 % of its design capacity and control valves are operating in a stable range. - Watch pH-value down streams of AN reactor. Try to operate permanently about a value of pH = 2 - 3, but always smaller than PH=3.5 (acidic range); undertake corresponding corrections. Check temperature of the TIAHL 31016/116 - Increase vacuum to approximately 0.33 bar abs - Watch temperature and pressure in vapor separator 31C001 - Start process condensate supply to the scrubber in 31C001 by FI 31407/457 - Start injection of water by FI31406/456 to vapor separator as soon as AN solution in 31C001 starts boiling. Adjust injection water quantity according to directive figures (see chapter "Normal Operation of the plant") - Check and watch permanently all important operating parameters and undertake corresponding corrections - Check and watch all control valves for proper function. - When approx. 25 30 % load of the plant capacity has been reached stop further increasing of plant load and adjust by manual operation the pH-value of ARCAHL 31701/751 to pH = 2,5 - Place controllers first of ARCA HL 31701/751 and after that of NH 3 gas flow control valve as well as of HNC flow control valve from "manual" to "automatic operation - Place all other controllers of the plant by and by from "manual" to automatic" operation as soon as the relevant operating parameters allows

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and the operating situation of the plant does not oppose - Check and watch for the initial start-up especially carefully the correct function of all elements and equipment of the plant during an operation period of at least several hours prior to - increasing the plant load to more than 30 %. - When everything is o.k. increase the load of plant slowly by and by in small steps up to 100 % by controller FRC 31403/453 of NH 3 gas flow control valve. Controller for HN0 3 flow will follow now automatically according to set point of pH-value on controler ARCAHL 31701/751. 1.3.2 Starting with demineralized water: If pure AN prills are not available, the neutralization start up will be with demin. water. When initially starting-up the AN-reaction system with demineralized water, all plant equipment is empty with the exception of AN reactor circuit which is to be filled with water and nitric acid. For this the demineralized water from water run, stored in 31 T001 will be pumped to the neutralization loop. After the water with nitric acid flow back to the tank via the overflow from 31R002, the start-up line will be closed, the pump 32 P004 stopped and the tank 31T001 drained. The whole equipment will be filled up during operation by the own AN production. The produced final AN-solution is weak in the beginning. The real initial start-up procedure of the AN-plant with demin. water is in principle the same as "starting with AN-solution". The procedure therefore is only roughly sketched here, since all detailed steps are to be applied according to its purpose and the statements as described for starting with AN solution. Following steps are to be executed for a start-up with demineralized water: - Fill AN-reactor circuit 31P001, 31R001, 31C001 partially with

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demineralized water and partially with - nitric acid giving a very weak nitric acid. - Start process condensate pump 31P005 - Start AN circulation pump 31P001 - Heat up the circulating weak solution by careful injection of heating steam via local flushing nozzles up to approx. 90 C; prevent "water hammering" - Just before start-up stop injection of heating stem - Add manually for some minutes ammonia gas in limited quantity. Check for concentration. Repeat this till circulating liquor is neutral - Start-up AN-reaction; prevent "water hammering"; Set on 30 % load - Decrease slowly the pressure in 31C001. In the beginning the produced AN-solution is very weak. By and by the circulating weak AN-solution is concentrated by the fresh produced AN, and the operating temperature increases and approaches to its design value. - Watch permanently the temperature of AN solution downstream of ANreactor . For detailed operating steps which are to be applied accordingly, see chapter starting with AN-solution

1.4 Vapor scrubbing and condensation:

Vapor scrubbing and condensation section of the plant is to be started up together with the neutralization section. Therefore the actions described here are also mentioned in the description of start up of the neutralization section in 4.1.3. 1.4.1 Preliminary operations: - Fill process condensate tank 31D001 with demin. water and start process condensate pump 31P005 - Fill demineralized water to 31D002 to have seal for condensers

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-Start ejectors 31A001 and 31A002 at open valves PV31213/313 with minimum steam pressure

1.4.2 Vapor scrubbing and condensation start:

- Start circulation of the process condensate through scrubber 31C001. Adjust flow to the scrubber by FI31407/457 at approx. 5 m 3 /h - Adjust vacuum in 31C001 by adjusting of the regulation valves PV31213/313 in steps to approx. 0.33 bar abs. - Adjust level in process condensate tank 31D001 and put LICAL 31504 on "automatic" - Adjust level in clean process - condensate tank 31D002 and put LICAHL 31505 on "automatic"

1.5 Ammonium nitrate solution tank:

AN solution tank is to be started up together with the neutralization section. Therefore the actions described there are also mentioned in the description of start-up of the neutralization section in 4.1.3. 1.5.1 Preliminary operation: For start-up of the neutralization as described in 4.1.3.1 AN solution must be prepared. If pure, uncontaminated AN solution with a concentration of 65 70 % is available, adequate quantity (approx. 50 - m 3 ) must be stored in tank 31T001. If ready solution is not available, it can be prepared from AN prills and demin. water. For preparation of AN solution only pure AN prills can be used, without any conditioning and coating additives. Before dissolution, the prills should be analyzed (total N content, H 2 O content, organic materials) and only if the results are satisfactory used for

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preparation-at-AN solution. Following steps are to be executed: - Fill approx. 20 m 3 demin. water in the tank 31 T001 and start heating with heating coils. - If the level in 31T001 is high enough, start AN heater pump 31P004 on circulation through AN circulation heater 31E003. - Set temperature control TRCAHL 31034 on about 80 C and place it on "automatic". - Check if temperature control valve as well as steam trap and steam condensate system are operating correctly. - Add about 50 tons of AN prills slowly into the demin. water in tank 31T001. - Circulate the solution through 31E003 till all AN prills are dissolved. 1.5.2 Operating: After the neutralization is started, AN solution tank adjustment must be corrected. - Check concentration increasing in the tank and increase temperature of the solution accordingly (up to 130 C) - Take ARCAH 31711 in operation and adjust the value of pH 5,0 - 5,5 - Observe temperature, concentration and pH indications during storage.

2. Granulation (Unit 32, 33, 34):

2.1 Solids system loading:
The here described sequence may immediately prolong the preparations in 3.2.2. (Sequence of start up see 3.2.2.9.) The granulation is loaded shortly before injection, after all equipment has been started up. Once the granulator is filled with solids and preheated, the production may

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start or the product may be cooled down and sent to the start-up bin again, according to the planning schedule.

2.1.1 Preliminary operations: Set splitter valve for on size material out of 32S004 to recycle conveyor belt 32H004. - Check clean status of start-up bin 32D001 and operability of start-up bin discharge activator 32H009. - Fill start-up bin 32D001 with AN prills over bucket elevator 32H003 through clean-out ports. - Start transfer of material from star-up bin 32D001 to the boot of bucket elevator 32H002 and to granulator 32 R001 via 32H004. 2.1.2 Granulator loading: - Adjust granulator scrubber exhaust fan 32 K004 to obtain a stable and gentle fluidization pattern during the loading operation which should be completed in ca. 15 minutes. - During the loading operation, fluid bed preheating may already be initiated with granulator fluid air heater 32E001/A to E until a bed temperature in chamber 2 of ca. 115 C is obtained while air temperature should never exceed 130 C. - Bring the solids level in 32R001 to at least 500 mm WC prior to slurry injection. - Compensate for dust losses if the bed is kept idle for several hours. Check scrubber operation/water balance/concentration to accommodate the AN

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dust recovery. - Scrubber circulation pumps are started up when the granulation -fans are in operation (mash plate).

2.2 Magnesium nitrate system:

2.2.1 Preliminary operations: - Start screw MgO 32H018. - Check dedusting of MgO bin 32D007. - Check MgO bin discharge activator 32 H013 and bin extraction rotary valve and stop both items. - Check dosing scale MgO 32H015. - Transfer an amount of ca. 5000 kg of MgO powder (in standard or big bags) to the MgO bin 32 D007 and calibrate the weight indicator. N.B. be careful that no rainwater nor bag debris enter the bin. - Check the status of the MgN solution cooler 32E005 of tank 32D008 as per 3.0. - Feed process water to MgN reaction vessel 32 D008 to a level equivalent to approx. 2500 l of water. - Start agitator 32N002. - Circulate water back to the vessel via pump 32P006 and one filter 32F001 with main discharge block valves closed and check water distribution in the overflow ring chamber. - Activate the pH analyzers and check their meters. - Steam flush and open the AN feed block valve and add enough nitrate solution (ca. 3000 l) to reach a solution concentration of approx. 50 %; then close the feed valve again and flush the line. - Simultaneously act on the cooling control to obtain ca. 70 C in the vessel (not more than 90 C). 2.2.2 Magnesium nitrate reaction: - Start the dosing Mg0 32 H015 at minimum accurate MgO flow.
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- Open the nitric acid block valve and adjust the flow in accordance with PH readings of ca. 2 (range 1 to 3). - Flush and reopen the AN feed . and check the ratio control with the nitric acid flow. - Proceed with reaction until the vessel level reaches the standard level gauge range, then stop, resp. start injection n to the AN solution heater according to planning.

2.3 Concentration system:

2.3.1 Preliminary operations: - Preheat the AN feed ring line by flushing with steam; all block valves at BL being closed. - Start AN circulation over the AN solution tank via the AN transfer pump 31P003. - Check closed status of the following block valves on the main feed line to AN-solution heater 32 E010: - Discharge of 32P006 from the MgN section of the plant; - Discharge of 32P004 from the dissolution vessel 32D004. - Activate tracing of mixing vessel 32D005 (mind boiling of residual water in the vessel). - Start filler mixing vessel agitator 32 N001. - Check if the seal in mixing vessel 32D005 is still filled with water. - Start pump 32P001 over slurry filter 32F002 and over recycle header back to mixing vessel 32D005. - Check status of the vacuum ejector 32A002 but keep its steam feed closed. - Preheat AN solution heater 32E010 with its steam feed (coil pressure at least 4 bar g) and steam flush (feed line, vacuum separator 32 C002, vapor line to vacuum condenser 32 E006 and down comer to seal of mixing

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vessel 32D005. 2.3.2 Concentration start: - Open AN feed block valve and start minimum flow with the control valve. - Adjust AN solution heater temperature to ca. 145 C and gradually activate the vacuum system to 0.5 bar abs to obtain a concentration of ca. 95 % . - Flush and start injection of MgN with pump 32 P006 according to further planning schedule. - Flush and start injection of recycle solution from 32 D004 according -to level requirements LRAHL 32519; mind plugging of injection line at how flow.

2.4 Slurry system:

2.4.1 Preliminary operations:
- Start screw filler 32H019 - Check weight of filler powder in filler bin 32 D002; bin extraction rotary valve and filler bin discharge activator 32 H014 having been checked prior to the start of the filler grinding system. - Check weighing system. 2.4.2 Filler addition: - Start filler flow to mixing vessel 32 D005 with liquid level well above the blades of mixing vessel agitator 32 N001. (Level LICAHL 32504 to be fixed during water run.) - Increase AN-solution heater cutlet temperature to ca. 168 C to increase concentration to 97 % (MgN included). - Start ammonia injection at inlet of the AN solution heater. Approx. 10 kg/w, metered by local FI32428 - Increase filler flow in ratio with the main An feed.

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2.5. Granulating aid system:

2.5.1 Preliminary operations: - Check level and temperature in granulating aid tank 32D013. - Start granulating aid metering pump 32P002 at minimum stroke; drain if necessary to avoid pressure buildup.

2.5.2 Granulating aid injection: - Open injection valve in the suction of 32 P001 and set required flow ratio but only seconds prior to the effective slurry injection in the fluid bed.

2.6 Slurry injection start:

This sequence may immediately follow the solids loading sequence 4.2.1., all the others sequences 4.2.2 to 4.2.5 being accomplished independently. 2.6.1 Ultimate granulator air system adjustment: - Open nitric acid/ammonia feed to scrubber circulation reaction vessel 32D003 and adjust pH balance. - Switch 32K001 to manual control. - Increase discharge pressure of atomization air blower 32K002 to ca. 0,4 bar g only seconds before effective slurry injection. - Increase 32K004 flow until granulator over pressure is corrected and switch 32K001 back to automatic. - Adjust atomization air temperature to 140 C by acting on heat exchanger 32E002. 2.6.2 Effective slurry injection: - Start slurry flow over the header of chamber 2 as per 1.3.4.3.1 with open recycle. -Adjust slurry pressure and start injection through individual headers II3

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and II2. - Close and flush main recycle header and adjust slurry pressure to ca. 1 bar g. - Start other headers as per 1.3.4.3.1.

2.7 Solids flow

- Start a small solids flow as soon as injection is operational while increasing granulator level to ca. 600 mm WC. - When granulator level reaches 600 mm WC, reset diverters under 32 S004 to allow the on size material to flow by gravity to 32E003 and to holdup bin 32D010. - Adjust dampers 32K003 and 32K005 to obtain a satisfactory material fluidization pattern with an overflow weir setting of ca. 10 cm. - Activate holdup bin extractor 32H008 after at least 5 minutes holdup delay to allow material feed to 32E007. - Adjust damper of 32K007, air recycle damper to 32K003 and damper of 32K005 to obtain a satisfactory material fluidization pattern with same overflow weir setting of 10 cm. - Adjust air temperature to reach the required material cooling pattern 55 C 40 C with first cooler air preheater 32E004 and final cooler air heater 32E009. - Check material flow to 32H003 and from there to start-up bin 32D001 via splitter valve. - As soon as the start-up bin contains enough fresh uncoated material, switch material flow to coating drum and to storage via conveyor belt 61H001.

2.8 Material coating (Unit 34):

2.8.1 Preliminary operations: The oil/amine system will be filled with oil/amine mixture just before

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start-un of the granulation plant. Before filling with oil/amine the whole system can be checked with oil or steam condensate/Demin. water. (If oil is used, the pipe system must be cleaned with steam after tests): - Fill the oil/amine preparation vessel, check LALH 34502 - Start 34 P001 on circulation and check FIQS 34401 - Start N001 and activate heating. Check TC 34003 - Fill 34D002 via 34P001, check LALSAH 34504 and TC 34010 - Start heating of the pipe system - Start the oil/amine metering pump 34P003 according to manufacturer instruction - Calibrate all pumps separately with spray nozzle disconnected by adjusting stroke. - Make sure that no syphonic through the pumps occurs (at stroke = 0 no flow) - Check set point and function of PIALSH 322371337 - Check SV 34010/020/030 - Check spraying nozzle for proper distribution and throughput - Check the function of drum heater 34E001 and amine barrel pump 34P002. 2.8.2 Coating start-up: - Activate heating and tracing - Supply and mix coating agent components at required ratio and temperature in oil/amine preparation vessel 34D001 - Flush injection line with plant air - Start oil/amine metering pump 34P003 with required stroke - Check spray pattern in the coating drum; switch pump or/and replace spray nozzle if nozzle dripping or sludge deposition is detected on the drum internals
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- Remember that spills of coated material may never be recycled; they must be collected as solids and discarded.

2.9 Dolomite grinding (filler):

Preparation for start-up and start-up of the dolomite grinding unit is to be done according to the "Erection, Operating and maintenance instruction" of the manufacturer (Indutec). (See para 1.2.4.)

2.10 End product output (Unit 61):

The end product is transported by conveyor belt 61 H001 to bagging or intermediate bulk storage. The conveyor belt - is equipped with a belt weighing system. The accuracy of such weighing is not sufficient for production / cost accounting but merely intended as , a trend indicator of the product output and as final check of the production split between the two parallel lines. Product must be sampled manually at the agreed periodicity and immediately poured in a closed sample flask. Since small product quantities are subject to rapid moisture uptake. The operator must take care to collect a fully representative sample from a chute and not from the top of the pile on the conveyor belt.

4.3 Summary of Start-up Steps:

Preparatory work for initial start-up 1. 1.1 1.2 1.3 1.4 all checks ready instruments air supply control circuits, control valves alarms, interlocking, trip system communications to interconnected plants (telephone, walky talky) power supply
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1.5 2. 3. 4. 5.

right position of valves; (generally closed, except instrument connections) cooling water running steam system under pressure NH 3 -evapcration under pressure preparation of AN-solution in tank 31T001

Start-up (preferably with AN-solution)

1. 1:1 Preparation Inform the partners of concerned plants resp. units upon forthcoming start-up, and make sure that they are prepared to supply their services resp. material continuously to the plant (cooling water, steam, instrument air, power, ammonia storage, nitric acid storage). .2 3 Raw materials, ammonia & nitric acid: block valves up stream of control valves closed, down stream valves open. All control valves closed; other than raw materials, adjacent block valves open; controller on manual operation, and setpoints on zero. 2. 2.2 2.2 Fill neutralization. Fill demin water in tank 31-D002, and also in tank 31-D001 to approx. 50 per cent, make sure water seal for vacuum. Preheat equipment of neutralization loop, and interconnecting piping, also start up line 50-AN-31 129, thoroughly by injection of steam through local flushing nozzles. 2.3 Start pump 31-P004, if not already running, and feed ANsolution from An-tank to suction line of AN-circulation pump

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3101-P001, and fill neutralization loop. 2.4 2.5 Start pump 31-PC05 to supply water injection to circulation pump 3101-F001 and to separator 3101-D001. After AN-solution has flown for a while into neutralizer 31R002 to ensure vacuum seal, start AN-circulation pump 3101P001. 2.6 2.7 Previously provide the seal of the pump by approx. 50 l/h of water. Stop filling, direct An-solution from pump 31-P004 through AN-heater 31-E003 to tank 31-T001 again. Set point of T RCAHL 31034 is 100 C for weak AN-solution (below 85 %) at initial start up, otherwise it is approx. 130 C 2.8 3. 3.1 Drain start up line 50-AN-31 129, and steam it out into weak solution vessel 31-D003. Start reaction. Start vacuum pumps 3101-A001 & 3101-A002. (Previously allow thermal expansion of NH 3-heater 31-E001 with only little steam). Then open steam valves fully. 3.2 3.3 Put pressure controller PRCAHL 31 213 or, automatic: set point 0.6 bar (absolute). Do not wait for reaching the set pressure Feed some steam into the neutralization loop through NH 3sepcrator 3101-DO05. Be cautious, avoid water hammering. Heat up AN-solution 3.4 3.4.1 3.4.2 3.5 Start pH-value measuring ARCAHL 31 701. Open demin. water, adjust quantity to approx. 70 l/h. Then add AN-solution in such quantity that temperature TIAHL 31016 of the resulting sample will stay just below 60 C. Check position of control valves and controllers according to pt. 1.2, then open block valves of NH, as well as nitric acid feed.
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3.6

Start pump 31-P006 for clean process condensate supply to the scrubber in 3101-D001 by Fl 31 407, charge it with approx. 2 m3/h. (The quantity of 5 m 3/h is adequate to 100% load; reduce it accordingly at reduced load.)

3.7 3.8

Override interlocking < 1 > for raw material feed. Open manually, gradually, and alternately in small steps the flow control valves of at first HN0 3 and then NH 3 . Watch pHvalues ARCAHL 31 701 downstream of reactor 3101-R001, and try to operate the control valves such that the pH-value is kept within the range of 2 - 3.

3.9 3.10 3.11 3.12 3.13 3.14 3.14.1 3.14.2 3.14.3 3.15 3.15.1 3.15.2

Go on until the plant load has reached approx. 25 %, where controllers can operate stable. Check AN-solution sample temperature TIAHL 31 016 and adjust AN-solution to 60 C, if necessary. Start injection of process condensate to vapor separator 3101D001 through FI 31 406, approx. 0.3 m 3 /h. Increase vacuum to 0.33 bar (absolute). Set pressure controller PRCAHL 31 213 accordingly. Stop steam injection into the neutralization loop (ref. 3.3). Put controllers on automatic: pH-value ARCAHL 31 701 set point 2.5 (Previously adjust as well as possible manually.) NH 3 feed FRC 31403 set point = actual flow Nitric acid FFIC 31 404 set point pH = 5.2. Open demin. water, adjust quantity to approx. 70 l/h. Then add AN-solution in such quantity that temperature set point = actual ratio Start pH-controller ARCAHL 31 703 and put on automatic:

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TIAHL 31 117 of the resulting sample will stay just below 60 C (provided level in neutralizer 31 RG02 is sufficiently high). 4. 4.1 Go on to normal operation. Activate interlocking < 1 % for raw material feed. Check all control valves for proper function. Check thoroughly all equipment, especially at initial start-up. 4.2 Put level controllers LICAHL 31 505 (tank 31-D002): set point 95 %, 5.5 m respectively, and LICAL 31 505 (tank 31D001): set point 50 % on automatic. 4.3 Open step-wise butterfly valve in vapor line 350-VF-31 603 to HN0 3 -heater 3101-E002, allow thermal expansion. Vent HN0 3 -heater. 4.4 If everything is o.k., increase load of the plant by and by in small steps up to 100 %, turning set point of NH 3 -controller FRC 31403, nitric acid flow will follow automatically. Watch actual pH-value remaining generally close to the set point. 4.5 4.6 4.7 Check instrument readings: see "Normal operation of the plant". NC T U SEE D. As soon as concentration of AN-solution in tank 31 T001 is higher than 85 %, set point of temperature controller TRCAHL 31034 shall be set on 130 C. 4.8 4.8.1 4.8.2 Start pH-controller ARCAHL 31 711 and put on automatic: set point pH = 5.2. Open demin. water, adjust quantity to approx. 70 l/h. Then add AN-solution in such quantity that temperature TIAHL 31 033 of the resulting sample will stay just below 60

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C.

Remarks for START UP SEQUENCE with water Preparatory work for initial START UP 5. Do not fill water in AN-solution tank 31-T001. START UP (procedure using demineralized water) 2. 2.2 2.3 Fill neutralization. DELETE Start pumps 31-P006 and 31-PC05 and fill demin. water through 3101-C001 into neutralization loop. 2.7 3.2 Pts. 2.4 to 3.7 replace "AN-solution" by "water in the loop". Stop filling, reduce flow through scrubber to approx. 0.5 m 3 /h (FI31 307). Put pressure controller PRCAHL 31 213 on automatic: set point 0.33 bar (absolute). Do not wait for reaching the set pressure! Delete pt. 3.12 accordingly. 3.3 Special attention has to be paid to this pt. Water hammering occurs more easily. Heat up until the liquor boils. Then reduce steam injection near to zero. 3.8 Special attention has to be paid to this pt. It is more difficult to keep the pH in the envisaged range of 2 - 3, also water hammering may occur. 4.6 As soon as level in AN-solution tank 31-T001 is above 5
79

% , start pump 31-P004 and pump liquor through AN-solution heater 31-E003. Put temperature controller TRCAHL 31 034 on automatic: set point is 100 C. Other points not mentioned above remain unchanged in comparison with the start-up procedure with AN-solution.

CHAPTER 5 NORMAL SHUTDOWN

1.General aspects 2. Normal shutdown of the AN neutralization plant
2.1 Less extended shutdown 2.2 Extended shutdown

3. Normal shutdown of the AN granulation plant

3.1 shutdown of a line in unite 32 3.2 Magnesium nitrate shutdown 3.1.1 Shutdown sequence .

4. power failure
4.1 unite 31 4.2 unite 32

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1. General aspects:
Normal shutdown is planned shutdown and Carefully prepared . the duration of shutdown is decided . it is done in case of required maintenance for an equipment .or annual shutdown , it is the most safe shutdown. Supply of raw materials must be informed by enough time the following three stages in duration of plant shut down shall be distinguished : 1- Short shutdown : raw material feed is shut off. 2- Less extended shutdown : AN solution is hold in the equipments for quick restart. 3- Extended shutdown : equipments is emptied to be sure not to block lines by crystallization.

1.1 The main operational aspects :

1.-The danger of freezing by crystallization with especially no flowing AN solution when cooling down in case of not being heated 2.-The draining and the time spending refilling works of the drained equipment units when starting again 3.-The mixture of the different equilibrium concentrations of the various AN evaporation stages when draining and starting up
81

4.With falsified concentrations.

1.2 Safety aspects to be considered :

1.-AN solution with a PH = 3.5 ,acid range .due to the danger of decomposition ,should possibly not kept in the plant equipments for a longer period 2.-Storing AN solution with PH = 4.5/5.5 alkalinity decreased into acidic range .

2. Normal shutdown of the AN-neutralization plant:

A normal shutdown is intended, regularly planned and carefully prepared, for this kind of shutdown ,in contrary to an automatic shutdown or an emergency shutdown, at the beginning the present plant load is gradually reduced in small steps. This has to be done slowly in away, that the NH 3-flow control valve and the HNO3 flow control valve have time to follow properly without larger deviation of the adjusted PH value . Thus the plant load will be carefully reduced up to the lowest possible operating point of approximately 30% of the design capacity, at which the NH3/ HNO3 flow control valves are gust still operating in a steady range . only when all necessary preparatory measures have been undertaken ,the positioner of PH controller ARCA31701 being still in automatic position ,the plant will be shutdown by pushing emergency shutdown button . to reduce the plant load below the stable operating point eventually by manual

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operation is too risky, since in the unsteady range there is no automatic control and proper indication for the PH-value, which really may permanently oscillate in wide range between acidic and alkaline operating condition.

2.1 LESS EXTENDED SHUTDOWN :

In this case the shutdown period not exceed 30 min circulation of AN solution through the loop . Above this time circulation is too risky due to temperature of solution will decreased 31013/113 and crystallization dangerous is possible , and there is no safe method for increasing this temperature . If trip 1 in temporary position is occurred or for temporary saving ammonia for the system of Abu Qir II less extended shutdown with circulation can be done as follow : 1.-The pump 31P001 is still in operation . 2.-Closing automatic valves of 31403/453 ,31404/454 and MV is not closed 3.-Opening PV 31213/313 . 4.-Stop steam supply to ejectors 31A001/A002 . 5.-Watch An solution temperature TR 31013/113 .it must never fall below 115 C . 6.-Continue the PH control and adjust accordingly ,the PH is not less than 4.5 7.-Decreasing level in 31D003 for preparation to complete shutdown if need .

2.2 EXTENDED SHUTDOWN :

If there is a problem in an equipment and maintenance will take time or a planned shutdown for any reason . shutdown of the line will follow this steps :
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1.-Decreasing level in tank 31D003 . by opening discharge of 31P008 to tank 31T001 . 2.-Check for drain of reaction loop , must be not blocked . 3.-Informing ammonia plant before decreasing load of the line . 4.-Deceasing load of the line gradually till 30% (NH3 in = 4 m3 /hr ) . with saving all operating parameters of operation in save values (temperature , ratio , PH ) , it is too risky to decrease the load under 30% . 5.-Put valves of ammonia ,nitric acid on manual position and close it completely ,and open the vacuum valve PV31213/313 6.-Closing MV of automatic valves 403,404 or 453,454 . and stop for circulation pump 31P001 . 7.-Closing steam valves on ejectors 31A001, A002 8.-Drain off AN solution from AN reactor circuit to tank 31T001 by the pump 31P008 . 9.-Close sample line and careful flashing for it . 10. -Vent of the ammonia feed lines to AN reactor 31R001, then the drain valve at the bottom of AN separator 31D005 is to be

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opened , if the drain valve is blocked or if AN solution is coming out 31D005 must be flushed by steam to be cleaned . 11.-Flushing condensate of reaction drain loop and 31C001 using opening vapor from

FV406/456,414/46 for cleaning of any crystallization separator . 12.-Flushing for nitric acid distributors to the reactor 31R001. 13.-Undertake all necessary measures to prepare the plant for quick restart up. inside

3. NORMAL SHUTDOWN OF THE AN GRANULATION PLANT:

Unite 32 contains solutions, slurries, solids .all main feed block valve include steam flushing /draining ,connections through there plug, all drain must be flushed and cleaned . = shutdown of one line in unite 32. preparation for shutdown done by reducing level in tank 32D004 , and level of 32C001 , informing NH3 plant for steam consumption saving 1.-Closing blocks of 403/453 ,404/454, 406/456 and AG injection . 2.-Closing TV011/111 completely and MV of the valve . 3.-Opening PV212/312 .,stop steam injection on ejector 32A002 . 4.-Drain off evaporator from the drain on 32D004 . 5.-Stop filler metering and mixing. 6.-Drain and flush tree group using steam 7 bar

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7.-Injection to 32R001 is still going on . 8.-When the pump 32P001 starts cavitations ,stop the pump and 32P002 9.-Isolating headers feeds 32R001. 10.-Drain off the pump and opening drain of 32D005,drain of F002,and the drains of individual ,main headers . 11.-Flush headers using steam 7 bar . 12.-Condensate flushing for mixing vessel 32D005 . 13.-Reducing atomization air pressure ,and increasing 14.-Switch manual the ,and fluidization granulator override extractor the air on level temperature, for cooling granulator slowly .

interlock for granulator empting . 15.-Empty hold-up bin 32D010 to zero .and drop the over flow wires 32 E003 ,32E007 . 16.-Isolating valves of 32042/142 ,32044/144 . 17.-Stop for blowers 32K003,K007,K005 . 18.-Closing drains of scrubber 32C001 to 32D04 . 19.-Reducing granulator temperature by valves 32023/123, 32016/116 . 20.-Stop for other equipments with avoiding interlock release . 21.-Stop for blowers 32K001, K002, K004 . of coolers

3.1 MAGNESIUM NITRATE SHUTDOWN:

Before normal shutdown of mg N reaction loop the level or mount of mg N must be consumed on both or one line till pump cavitation 32P006 with consideration
86

of 100% level =18m3 mg N ,and consuming the weight of mg O on small bin . to be cleaned with service air after stop closing . 3.1.1 Shutdown sequence . 1.-Stop nitric acid feed 32 401 and close block valve . 2.-Stop mg O closing . 3.-Stop AN feed , close block valve , and drain flush through open control valve 32 402 (override ) . 4.-Check cooling system on mg O reaction 32E015 , and automatic valve . a.TV 32 001 A b.TV 32 001 B 0.0 % 100 % . vessel 32 D008 to maintain temperature at least 70 C by closing the path on cooler

4. POWER FAILURE :
All equipments is stopped , supply of steam is shut off ,all vents must be drained and flushed and lines also ,actions must be quick enough to avoid blocking .

4.1 Unite 31:

a.-Drain off neutralization loop to D003. b.-Closing MV , quick drain and flushing for lines .

4.2 Unite 32:

a.-Opening drains of individual headers ,and MV of headers in position of operation ,then little flushing of it . b.-Opening doors of granulator R001 and flushing of the bed using condensate . c.-Opening drains of D005, F002, P001 . d.-Drain off concentration section feed lines E010 and flushing with steam remaining in the system .

87

e.-Opening manholes of all blowers . f.-Opening drains of atomization air, fluidization air ducts . g.-Flushing of D005 ,P001 ,discharge line to R001 . h.-Isolating block valves feeds 32D008 ,flushing of AN line 402. i.-Closing MV bottom of D008 ,and drain for suction line ,P006 discharge line ,filter F001 .

Chapter 6 Normal operating parameters

1. General aspects 2. Most important operating parameters 3. AN neutralization plant
3.1 Ammonia evaporation and vapor condensation 3.2 AN neutralization 3.3 AN storage tank 3.4 Analysis sheet for AN solution U 31.

4. AN granulation plant
4.1 MGN preparation 4.2 Slurry concentration 4.3 Fluidized bed granulation 4.4 Product cooling 4.5 Scrubbing 4.6 Steam and condensate system 4.7 Analysis sheet for AN granules U 32.

5. Maintenance
5.1 Civil maintenance 5.2 Instrument maintenance
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1. General aspects
During normal operation the plant is operated automatically to a large extent by virtue of the installed control instruments to keep the plant running smoothly for making a satisfactory production in quality as well as in quantity , following advice should be observed and taken into consideration . The operation of the plant should continuously be under taken routine inspection , the automatic control instrumentation should be considered as a help in operating the plant , but it does in no case replace careful and critical supervision by the operating personal . Therefore all important physical and chemical operating data are permanently to be checked and critically watched . Continuous routine chemical control of the plant in accordance with chapter 2 sampling schedule are also indispensable . If it seems necessary or useful adjusted instrument set point for trips and alarms have to be received immediately in case of operation experience mode . A routine registration of the stated operating data is a good practice , if it is not done habitual , uncritical , routine way , the operators should rather compare and check in critical way the stated data with the nominal data . Already relatively small unmoral deviations between the effective and nominal operating parameters should be tired to be compensated by relevant small operating regulations . In case of serious irregularity in operation , the competent
89

operator should immediately inform the shift engineer before the operation runs the risk to get out control . It is evident that all relevant safety instructions and rolls for prevision of accidents must always strictly be observed .To avoid accidents the plant should always be kept in clean condition . Leaks even small ones particularly in pipe work and equipments carrying ammonia , nitric acid , or AN solution should be tightened as soon as practicable to avoid damage and to protect the operating personal . Spilled acid should at once be washed away with penalty of water or should be neutralized with soda ash . spilled AN solution should be washed away with penalty of water only if its contaminated , clean solidified melt can be put into the granulation loop .

2. Most important operating parameters :

For normal operation under design condition at 100% load the following most important operating parameters for the process units should specially be observed

3. AN neutralization plant: 3.1 NH3 evaporation and vapor condensation .

oInstrument : LICAHL- 31501. oService : NH3 in 31E006 . oNormal range : 20 60 % . The level of NH3in 31E006 is adjusted by LV31501 . level of evaporator affected pressure before PV31207 , increasing level increases pressure . In case of low pressure the level must be increased to compensate pressure decrease . But stripping to 31E007 is required . and check cooling water inlet temperature . the level mustnt reach to 100% because LV31501 will closed by trip link , to avoid AL enter to the system .

Instrument : PICAL-31207 Service : NH3 feed to reactor .

90

Normal range : 3.5 3.8 bar .

Pressure of ammonia gas must be at normal rang . to insure accurate reading of FV of AG to 01/02 R001( to be in the rang of P&T compensation equation of controllers) . and to avoid the effect between it and pressure of the reactor . Instrument : PIAL-31211 . Service : HNO3 at B.L . Normal range : 6 8 Bar .

HNO3 inlet pressure affected by level in HNO 3 storage tank . high pressure inlet E002, may affect pipes of the heater , and to avoid opening of safety valves of E002 . ( 9.5 Bar ) . Low pressure affect plant load due to large opening in valves 404 / 454 , not enough to reach the required elevated load of the plant . So the pressure must adjusted at satisfied value (6-8 Bar ) .

Instrument : PRCAHL 31213/31313 . Service : vapor from 31C001 . Normal range : 0.31 0.35 Bar .

Pressure of C001 is affected by temperature of reaction loop , and werng ratio , and concentration of nitric acid from B.L . Deviation of pressure need chick for ( wrong ratio , temperature of the reaction , PV213/313 , concentration of HNO3 , MV to atmosphere ) . high vacuum lowers the temperature of the reaction and increase concentration .

Instrument : T1 31002 . Service : NH3 in 31E006 . Normal range : 15 16 C .

Temperature of NH3liquid changed with the supply ( NH3 plant or NH3storage U.81 ) . This temperature affected the pressure inside evaporator and some factors can treat the deviation . ( temperature of cooling water , stripping to 31E007 , level inside 31E006 ) .

91

Instrument : TI 31007 . Service : NH3 After 31E001 . Normal range : 55C .

This is the temperature of NH3 gas enters to the reactor , it will effect on the temperature of the reactor ( R001) . The amount of the steam driving ejector and vapor is the heating medium , if this amount decreases the temperature 31007 will decrees .Chick for steam valve on 31E001is needed , the valve can be used at critical case , such as start up difficulties .

Instrument : TI 31014/114 . Service : Vapor from 31C001 . Normal range : 71-80 C

Temperature of vapor is followed as indication of reaction loop condition , and its affect the amount of incondensable gases that will be used in heating NH3gas enters the reactor .

Instrument : TI 31009/109 . Service : HNO3 after 31E002 . Normal range : 55 C.

Temperature of NA affect temp . of the reaction inside the reactor .and deviation need chick for temperature of NA from BL , temperature of 014/114 .

Instrument : TI 31037 . Service : H2O outlet 31E006 . Normal range : 37 41 C .

Cooling after outlet temperature compared with inlet temperature , the difference always (2-3)C at normal running of the plant .

3.2 AN NEUTRALIZATION

Instrument : ARCAHL 31701/751 . Service : PH reactor loop .

92

Normal range : 2-3 .

Reaction medium is acidic medium to inforce the temperature to go . so excess reactant is nitric acid and enter the reactor first to acidify the medium of circulated AN to be react with ammonia , and the outlet PH = 2-3 . Any deviation from instrument and laboratory analysis adjusting the flow of 403/453 , 404/454 will solve the problem .

Instrument : FRC 31403/453 . Service : NH3 to reactor . Normal range : 13.3 m3/hr .

Following reading of NH3 valve must be done because ammonia flow is the effective in ratio loop , the small flow compared with 404 flow .Any oscillation changes the ratio sharply and may cause ratio trip of the line , the amount of ammonia feed affect on vacuum and PH of reaction loop .

Instrument : FIC 31404/454 . Service : HNO3 to reactor . Normal range : 48 -49 C .

HNO3 flow in depended on concentration of N.A feed , the flow increased to adjust reading of 701 about 2-3 PH in order to composure concentration deviation.

Instrument : FI 31407/457 . Service : washing condensate . Normal range : 4-8 m3/hr .

The flow of washing condensate on trays of vapor separator to insure good washing of vapor leaving C001 , High or low flow is not recommended.

Instrument : FI 31406/456 . Service : saturation condensate . Normal range : 3.2 m3/hr .

It is considered as the pre scrubbing stage , normal flow of 406 will saturate

93

vapor to be scrubbed with respect to higher flow will affect temperature of 013/113 .

Instrument : TIAHH 31011/111 Service : AN after 31R001 Normal range : 150 C .

The temperature alarm on 155 C quick treatment for temperature adjusting t ratio of feeds and temperature of 013/113 before trip signal at 160 c that will stop the line .

Instrument : TIAHL 31016/116 Service : PH reactor loop Normal range : 60-70 C

The temperature must be adjusted to insure good reading of PH analyzer and avoid damage of electrode .

Instrument : TR 31013/113 . Service : AN in 31COO1 Normal range : 118 C

The temperature of 013 is the indicator of many parameters as ( vacuum , reaction condition , cond. flow ) .

Instrument : ARCAHL 31703 . Service : PH neutralizer Normal range : 5.0 5.5 . Instrument : TIAHL 31117 . Service : PH neutralizer Normal range : 60 - 70 C

Check on AG enters to the neutralizers .

The temperature must be adjusted to insure good reading of PH analyzer and avoid damage of electrode .

3.3 AN STORAGE TANK :

Instrument : ARCAHL 31711.

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Service : PH in 31T001 Normal range : 7 .

AN when stored the PH of AN must be in the range above acidic medium , to avoid chance of the decomposition of AN . Amount of AG is opened on the tank to adjust PH at 7 .

Instrument : LIAHL 31509 . Service : AN in 31T001 . Normal range : 20 % .

Adjusting load of units 31, 32 , to keep level of tanks in normal range , and it must be not less than 16 % .

Instrument : TRCAHL 31034 . Service : AN outlet 31E003 . Normal range : 130 - 135 C

Heating of AN stored in the tank is done by two methods : 1.Circulation on E003 2.Heating by using big and small coil inside the tank . Temperature of the tank should be in the range of 130 C , the temperature of 034 is ( 130 135 C ) . Crystallization of AN is a big problem .

Instrument : TIAH 31030 . Service : AN in 31T001 . Normal range : 125-130 C .

Temperature alarm on high temp to maintain AN on required position . High temperature need to adjusting the temperature of 034 and chick steam coil on the tank .

Instrument : TIAHL 31033 . Service : PH sample . Normal range : 60 - 70 C .

The temperature must be adjusted to insure good reading of PH analyzer and avoid electrode damage .
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Instrument : TIAH 31043/44 . Service : AN transfer pump . Normal range : 130-135 C .

Temperature on pump 31P003 A/B must not higher than temperature of 030 . If this takes place change over the pump from A to B or B to A to check the pump carefully .

3.4 ANALYSIS SHEET FOR AMMONIUM NITRATE SOLUTION . U . 31

VAPOUR CONDENSER FROM 3101 E005 AE 31708 PH A.N. Mg / L 2.5 3.8 N.D Free NH3 mg / I < 40 Free HNO3 mg / I <150

VAPOUR CONDENSER FROM 31102 E005 AE 31707 PH A.N. Mg/L 2.5-3.8 N.D Free NH3 mg /L <40 Free HNO3 mg /I <150

CLEAN PROCESS CONDENSATE TANK 31 D002 AE 31706 PH A.N. Mg/L Free NH3 mg/ L Free HNO3 mg /I

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2.5-3.8

N.D

<40

<150 Process Water Pump To Unit 32

PROCESS CONDENSATE TANK 31 D001 Process Water Pump To Unit 21 PH Free HNO3 Mg/L 1.4-2.2 PH 2 - 3.5 PH 2 - 3.5 PH 6-7 PH 6-7 AN % 90-93 % AN SOLUTION TANK 31T001 AN % 90-93 % <25000 A.N. mg /L <3000 1.5-2.3 PH

Free HNO3 mg/L <23000

A.N. mg /L <3500

REACTOR 3101 R001 Free HNO3 ( Mg / L) <3500 REACTOR 3102 R001 Free HNO3 ( Mg / L) <3500 NEUTRALIZER 31R00

4. A.N Granulation Plant U 32 :

4.1 MgN Preparation:

Instrument : ARCAHL 32 701. Service : PH in 32 D008 . Normal range : 0.8 1 . Instrument : FRAHL 32 401 .

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Service : HNO3 Flow to 32 D008 . Normal range : 2 2.5 m3/h . Instrument : FRAHL 32 402 . Service : AN Flow to 32 D008 . Normal range : 1 1.5 m3/h . Instrument : FRCAHL 32 403/453 . Service : an to evaporation . Normal range : about 39 t/h . Instrument :FRAHL 32 404/454 . Service : MgN to evaporation . Normal range : about 2.2 t/h . Instrument : TIC 32001 . Service : temp in 32 D008 . Normal range : 70 90 C . Instrument : TI 32 073 . Service : cooling water inlet 32 D008 . Normal range : min 45 60 C . Instrument : WICAL 32 802 . Service : MgO to 32 D008 . Normal range : about 400 450 kg/h .

4.2 Slurry concentration:

Instrument : TICSAH 32 011/111 . Service : temp in 32 C002 . Normal range : 165 - 170 C . Instrument : TICAHL 32 012/112 . Service : Temp in 32 D005 . Normal range : 165 175 C . Instrument : PICAHL 32 212/312 .

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Service : Pressure in 32 C002 . Normal range : 0.5 0.6 bar a . Instrument : PRC 32 213 /313 . Service : pressure inlet granulator . Normal range : about 2.5 bar . Instrument : WFIC 32 811/861 . Service : Dolomite to 32 D005 . Normal range : about 1200 kg/h .

4.3 Fluid bed granulation:

Instrument :LRCAHL 32 508/558 . Service : granulation level . Normal range : about 600 700 mm WC . Instrument : TRCAL 32016/116 . Service : atomization air . Normal range : 140 145 C . Instrument : PISAL 32217/314. Service : atomization air . Normal range : 1.2 1.5 bar a . Instrument : TRC 32022/122 . Service : temp in 32 R001 . Normal range : 125 130 C . Instrument : TIC 32 023/123 . Service : fluid . air temperature . Normal range : about 100 C .

4.4 Product cooling:

Instrument : LICAHL 32511. Service : NH3 in 32 F004 . Normal range : 30-70 % .

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Instrument :TIC 32044/144 . Service : air inlet 32 E007 . Normal range : about 25C to have granules cutlet temperature of about 40C ( TLC 32043/143 ) . Instrument :TIC 32 042/142 . Service : air inlet 32 E003 . Normal range : to have granules outlet temperature in range 50-60 C ( tic 32041/141 ) .

4.5 Scrubbing:

Instrument :AIC 32704/754 . Service : PH in 32 D003 . Normal range : 7-8 . Instrument :TIC 32062 . Service : solution in 32 D004 . Normal range : 40-50 C . Instrument : FICAL 32429/479 . Service : pewetting inlet 32 C003 . Normal range : 5-10 m3/h . Instrument : TICAHL 32060/160. Service : prewetting inlet 32 C001 . Normal range : 40-75 C .

4.6 Steam and Condensate System:

Instrument :PICAL 31251 . Service : steam after 31 E008 . Normal range : about 12 bar a . Instrument : PICAHL 31254 . Service : steam after 31 E009 . Normal range : about 7 bar a .

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Instrument :TICAH 31021. Service : steam after 31 E008 . Normal range : 190-200 C . Instrument : TICAH 31024 . Service : steam after 31 E009 . Normal range : 165-175 C .

4.7 ANALYSIS DATA FOR A.N. GRANULATION UNIT U 32

Production to storage from line .
Bulk TIME T.N % WT Ca % WT Mg.N % WT >= 1.6 Moist % WT =< 0.5 Density Kg/m3 960 Hard K.P 3.0 PH 10% 6.6

>= 33.0 >= 0.05

Screen analysis ( %WT )

TIME >4.5 mm >= 33.0 4.0-4.5 mm >= 0.05 3.15-4.0 mm >= 1.6 2.0-3.15 mm =< 0.5 < 2.0 mm 960 2.0-4.5 mm 3.0

Mg.N Reaction Vessel 32 D008

TIME PH 0.9 Mg.N % WT A.N % WT 29 %

29 %

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Scrubber Circulation Reaction Vessel ( 3201D003 )

TIME 32 704 I PH 8 % A.N 32 704 II PH % A.N 8

5.1 Civil maintenance:

The civil Engage Dept regularly checks the roofs , walls and floors of the building . Special attention should be paid to : a.Any corrosion of concrete from nitrate solution . b.Any corrosion of the sealing seam sin acid resistant floors . c.Broken tiles and seals in all acid resistant floors , cracks in bitumen layers . d.Any such damage should be repaired without delay .other maintenance work on buildings depends on the circumstances e.In most cases it is done at the request of the production people f.Never place heavy materials on a tiled floor , but use a load spreading intermediate platform . g.Broken tiles should be replaced immediately , to avoid decay of the floor base , this also applies to damage asphalted floors h.Avoid hot condensate of product splashing in to the floors since this may cause the concrete to deteriorate .

5.2 Instrument maintenance:

(periodical maintenance )
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Instrument Pressure transmitters Level transmitters calibrate Inductive flow transmitters Rota meters calibrate P-cells Temperature transmitters Thermocouples Mel volt recorders check Analysis meters Controllers recorders Indicators (pressure, temperature ) control valves relays switches should be doubled .

Frequency every other year every other year every other year every other year once a year once a year every 6 months every 3month every other year one in 3 years once in 3 year once a year once a year

Action calibrate check, overhaul calibrate check overhaul check o-point calibrate change thermocouples lubricate ,calibrate check , overhaul Calibrate and indicators calibrate check overhaul check , calibrate check

see instructions of apparatus

for instrument , relating to guarantee measurements , the frequency

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Chapter 7 SAFETY INSTRUCTIONS

1. General 2. Ammonium nitrate (NH4 NO3). 3. Ammonia(NH3). 4. Nitric acid(HNO3). 5. Nitrous gases. 6. Oil/amine solution. 7. Granulating aid. 8. Protective equipment.
8.1 General measures to reduce the danger of accidents.
8.1.1 Special measures to prevent accidents when working on electrically driven equipment and machinery.
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8.1.1.1 Special measures to prevent accidents during sampling. 8.1.1.2 Special measures to prevent accidents while opening and inspecting vessels and equipment. 8.1.1.3 Special regulations for the inspection of vessels, equipment etc. 8.1.1.4 Special measures to prevent accidents during welding works:

9. Fire protection devices.

9.1 Fire fighting.

1. General:
The guiding principles for safety contained here in are extract form official regulations of particular importance. These principles are therefore by no means complete, and the relevant regulations for the prevention of accidents should be studied in conjunction with them.

2. Ammonium nitrate (NH4NO3):

In general: ammonium nitrate hardly irritates human skin. However, usually it is used in form of a concentrated solution at correspondingly high temperature. For this reason, there exists a particular danger of burns. Pure ammonium nitrate or high-concentrated ammonium nitrate melts can explode in case they are entrapped and subject to increased temperatures over extended periods, so that a certain pressure may form up. Ammonium nitrate is sensitized due to its explosiveness by several inorganic and organic substances, mostly reducing, but also by chlorides. Ammonium nitrate does not have any specific occupational health problems. The dust arising from ammonium nitrate (or CAN) is of low toxicity and is generally
105

regarded as a nuisance dust with 10mg.Nm -3 (8 hour exposure) being accepted as the permitted level provided the particle size is above 5m. Ammonium nitrate may decompose in a fire situation and thus stores should be suitably designed with consideration for factors such as access to stacks, spacing between stacks, presence of other chemicals (such as combustible materials). Oxides of nitrogen will be emitted during a decomposition.

UNIT - 32
The main chemical hazards associated with ammonium nitrate are:- Fire Decomposition Explosion Burns caused by hot AN solution should also be considered from a safety point of view. Fire Ammonium nitrate itself does not burn. Being an oxidizing agent, it can facilitate the initiation of a fire and intensify fires in combustible materials. Hot AN solution can initiate a fire in rags, wooden articles etc., on coming into contact with them. Similarly, fertilizer products or dust contaminated with oil or other combustible materials can also start fires when left on hot surfaces. Fires involving AN cannot be extinguished by the prevention of air ingress (e.g. smothering with steam) because of the provision of oxygen from the AN. Decomposition Pure solid AN melts at 169C. On further heating it decomposes by way of a complex set of reactions. Up to about 250C it decomposes primarily into N 2 O and H
2

O. Above 300C reactions producing N

, NO, NO

etc., become

significant. These reactions are exothermic and irreversible. They are accompanied by the vapor pressure dependent endothermic dissociation into
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HNO 3 and NH 3 vapors which can provide a temperature limiting mechanism, provided the gases can escape freely. If they cannot, the endothermic dissociation is suppressed and a run-away decomposition can develop, leading to explosive behavior. A number of materials have a strong catalytic effect on the thermal decomposition of AN. These include acids, chlorides, organic materials, chromates, dichromates, salts of manganese, copper and nickel and certain metals such as zinc, copper and lead. The decomposition of AN is suppressed or prevented by an alkaline condition. Thus the addition of ammonia offers a major safeguard against the decomposition hazard. The release of toxic fumes is one of the main hazards associated with the decomposition of AN. Explosion AN is especially difficult to detonate and neither flame, spark nor friction is known to cause detonation. Shocks derived from detonating gas mixtures (hydrogen/oxygen or acetylene/oxygen) have been found to be incapable of producing detonation in AN. AN fertilizer dust, being non-combustible in nature, does not give rise to a dust explosion such as those commonly associated with grain and organic dusts. Shock initiation in solid prilled AN needs a fairly substantial stimulus. Heating under confinement and shock initiation of hot or contaminated AN by projectile impact appear to be more credible mechanisms in the context of industrial operations. Strongly acidic conditions and the presence of contaminants should be avoided to counter the explosion hazard in AN solutions. Explosions can occur when ammonium nitrate is heated under confinement in pumps. Reasons for pump explosions include:- No (or insufficient) flow through the pump Incorrect design (Design may incorporate low flow and/or high temperature trips) Poor maintenance practices
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Contamination Burns Caused by Hot AN Solutions These solutions are dangerous because of their high temperatures (commonly in the range 120-180C) and because they attack the skin on account of their oxidizing properties.

GENERAL PRODUCT INFORMATION ON AN GRANULES

Identification: Chemical name : Commonly used synonyms : Molecular formula : Ammonium Nitrate AN, Ammonium Nitrate Fertilizer NH 4 NO 3

Hazards to Man and the Environment:To man: Ammonium nitrate is basically harmless when handled correctly. To the environment: Ammonium nitrate is basically harmless when handled correctly. Physical and Chemical Properties:Appearance : Odour : Melting point : Boiling point : White or off-white granules or prills Odour less

PH water solution (10g/100ml) :- >4.5 160-170C depending on moisture content >210C (decomposes by dissociation)

Explosive properties : Not explosive as The fertilizer has a high resistance to detonation. This resistance is decreased by the presence of contaminants and/or high temperatures Oxidizing properties : Can support combustion and oxidize. Not classified as oxidizing. Solubility in water : 1,900g.l -1 at 20C

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Bulk density :

830 to 1,100kg.m -3

UNIT 31 Guidance for the storage of hot Ammonium Nitrate solution:SCOPE AND PRINCIPLES: This guidance concerns the storage of hot ammonium nitrate solutions with a concentration in excess of 80% in fixed tanks. The recommendations are not intended for tanks used as process vessels in manufacturing plants. This guidance may also serve to determine the basic safety concept in performing safety studies and the design of storage tanks related to hot ammonium nitrate solutions. This guidance is intended to apply to new installations but consideration must be given to adapting existing installations wherever reasonably practicable. It must also be borne in mind that not all recommendations may apply in every situation and retrofitting or modifying existing installations may not always be possible from a technical or practical point of view. In such cases appropriate safety studies should be carried out to establish that the existing situation is acceptable. The guidance is not prescriptive in nature but provides a series of recommendations. It attempts to describe the relevant factors , their relative importance and various options available to specific situations. This guidance addresses various safety related aspects of the storage of ammonium nitrate
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solutions. The guidance briefly describes the physical and chemical properties of AN, focusing on the potential hazards of hot AN solutions. It also covers the main regulations, which apply to the production and storage of hot ammonium nitrate solutions in the European Union. Readers are advised to refer to up-todate regulations as there may have been changes since the publication of this guidance.

The properties of hot concentrated solution of AN: 1. Physical Properties Ammonium nitrate is very soluble in water. Heat is absorbed when it dissolves, which makes the process of dissolution difficult and slow at low temperatures. The crystallization temperatures as well as the atmospheric boiling points of AN solutions of different concentrations are given in the table on next page.

More detailed information regarding the relationship of atmospheric pressure boiling and crystallization temperatures of AN solution is given in Diagram 1.

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2. Chemical Properties Hot AN solutions should always be stored under neutral or alkaline conditions. It is common industrial practice to express the pH of an AN solution as that of a 10 wt% solution at 25C. According to this practice the pH of a neutral AN solution is not 7 but is in the region of 4.5. Measuring the pH at different concentrations and/or temperatures will result in different values and these values need to be appropriately adjusted. AN solutions themselves are neither combustible nor flammable. They are oxidizing in nature and thus can enhance the potential fire hazard of combustible material. They can react on contact with organic materials such as wood, oil or grease, in some situations after a delay. Hot AN solutions are capable of thermal decomposition conditions. Decomposing ammonium nitrate solutions can evolve N 2 O, brown nitrous fumes (NO x ), nitric acid vapors and NH 3 , some of which are toxic in nature and, therefore, should not be inhaled. Whereas most of the decomposition reactions are which is negligible under normal storage

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exothermic in nature, the dissociation reaction (into ammonia and nitric acid) is endothermic and is vapor-pressure-dependent. The tendency to decompose is enhanced by high temperature, acidic conditions and the presence of contaminants containing ions of, e.g. Cl2, Fe, Co, Ni, Cr, and Cu. AN solutions also react vigorously with zinc and zinc alloys (note that zinc is widely used in galvanized steel). Once started, these reactions can become progressively more severe, unless controlled. In this guidance the two types of reactions, decomposition/ dissociation and oxidation, are described simply as decomposition. Hot concentrated AN solution can give rise to a potential explosion hazard when heated under confinement (e.g. in a blocked pipe) or by severe shock derived from a high explosive or a high velocity projectile.

3. Environmental Aspects Ammonium nitrate has a low toxicity to aquatic life. It is the free or non-ionized ammonia generated due to the dissociation (which tends to be small) of AN, which produces the toxic effects. Ammonium Nitrate is a nitrogen fertilizer. Heavy spillage may cause an adverse environmental impact such as eutrophication in confined surface waters, or nitrate contamination. AN is biodegradable and does not show any bioaccumulation phenomena. 4. Health Hazards In respect of people, AN is generally considered to be of low

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toxicity through all major absorption routes. Hot concentrated solutions of AN can produce very severe burns on the skin. This is not only because of their high temperature but also because they attack the skin on account of their oxidizing properties. First aid details are given below. A toxic hazard can arise from brown nitrous fumes given off by decomposing ammonium nitrate solutions. These fumes must not be inhaled and they can have an insidious and delayed effect Protective measures should be taken in case ammonia is present in the area near the storage tank, for example, due to overammoniation and local venting.

GENERAL PRODUCT INFORMATION ON HOT AN SOLUTION

Identification: Designation: (80-93%). Ammonium nitrate, hot solution in water

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Trade name Commonly used synonyms: Ammonium nitrate solution (80-93 weight %). Intended use: Raw material for production of fertilizers, explosives and nitrous oxide. Hazards to Man and the Environment: These solutions are dangerous because of their high temperature and because they attack the skin on account of their oxidizing properties. Skin Contact: Eye Contact : Ingestion: This event is most unlikely because of high temperature of product. However, small quantities of ammonium nitrate are unlikely to cause toxic effect. Large quantities may give rise to gastrointestinal disorders and in extreme cases, formation of methaemoglobin (blue baby syndrome) Inhalation: and cyanosis (indicated by blueness around the mouth) may occur. Mists and low concentrations of ammonia released from the hot solution may cause irritation of eyes, nose, throat and upper respiratory tract. Long term effects: No adverse effects are known. Physical and Chemical Properties: Appearance: Color less clear liquid when free
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Hot material will cause thermal burns. Hot splashes will cause eye burns and

permanent eye damage.

from crystals. Odour: between 5 and 7). Freezing point: 93% AN. Boiling point: 93.0% AN. Vapor pressure at 100C: 39.6kPa (80% AN); 22.6kPa (89.9% AN). Explosive properties: can lead to a violent reaction or explosion. Not classified as explosive. Solubility in water: Density: AN). Protective measures: Large amounts of high-concentrated melts may only be heated up above 160 C for a very short time (some few seconds), e.g. locally in heat exchangers etc. Ammonium nitrate should not come into contact with combustibles, i.e. organic materials. Any ammonium nitrate which may step out of the system should be carefully cleaned off. Free acid contents in concentrated ammonium nitrate solutions and in the presence of chloride ions will favor a decomposition at increased temperatures. Therefore, a slight surplus of free ammonia in ammonium nitrate solutions is recommended,
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Weak ammonia odour.

PH water solution (conc. 10% AN): > 4.5 (for transport, pH must be 96 C at 90% AN, 110 at 146 C at 90% AN; 159C at

Heating under confinement

Miscible in all proportions. 1.41g/cm 3 at 100C (91%

clocked lines are to be opened by means of slightly warm water. Welding work on systems which transport pure ammonium nitrate or in form of mixtures should not be carried out before the systems have been thoroughly cleaned. These are only filled again when the spot concerned is cooled down to the ambient temperature. Persons working on piping or vessels containing ammonium nitrate must always wear protective goggles and gloves, the attar for protection against heat . First-aid measures: Skin contact:In case of burns due to hot ammonium nitrate solution the

corresponding spot stall be flushed with large quantities of water and if required, shall be treated according to the instructions for usual burns. Eye contact:If the eyes are affected, these must be washed out with clean

water and thereafter. medical assistance should be called for.

3. Ammonia(NH3):
Under normal circumstances, ammonia is a colorless gas and is lighter than air. It is easily recognizable by its extremely pungent odour. Ammonia is easily liquefiable under pressure. At atmospheric pressure, ammonia will evaporate at a temperature of about -33 C, while absorbing heat from ambient matter. Ammonia is easily soluble in water; such solutions can contain up to 35 % ammonia(ammonia water). Liquid ammonia, high-percentage ammonia water and highly concentrated gaseous ammonia will irritate human skin and cause severe burns .Gas of high concentration will paralyze respiratory organs.

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The following are particularly endangered: a) Eyes b) Mucous membranes (mouth, throat, respiratory ducts, lungs, genitals) c) Larynx, gullet and stomach, particularly if aqueous ammonia solution is swallowed. Injuries to the larynx and lungs can be fatal. The pungent odour is an adequate warning and will therefore prevent severe injuries to health, since the real danger begins when the endurability limit is exceeded. The maximum permissible concentration in a working area over eight hours is approx. 50 ppm, equivalent to 35 mg/rn3. Irritation of the larynx and the eyes will become noticeable when the concentration is ten times as great. At an ammonia concentration of 0.15 %, uncontrollable coughing will set in, and at a concentration of 0.5 % paralysis of the respiratory ducts will begin. Concentrations of around 2 % will perceptibly irritate uncovered skin. If liquid ammonia comes in contact with human skin, there is a danger of under cooling . Great care should be exercised when handling ammonia. A mixture of air and ammonia can be explosive. This is particularly the case, whenever the ammonia content of air at normal temperatures and pressures is from15.5 to 27 % by vol. In the presence of other combustible substances, such as hydrogen or acetylene, at higher oxygen contents of air or at abnormal pressures and temperatures, the hazard limits will cover a greater range, thus the danger
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will be bigger. Explosive mercury compounds (acids) may form if compressed ammonia bearing gases come in contact with metallic mercury. Thermometers, pressure gauges, and the like installed on ammonia-bearing equipment or piping should therefore not be of the mercury type.

Protective measures: Whenever ammonia is escaping from a piece of equipment or a pipe, the room must be evacuated at once, using gas masks. The endangered zone should be thoroughly ventilated as soon as possible. In view of the fact that ammonia is lighter than air, ventilation by upward draught will be most effective. If any work has to be carried out in rooms contaminated with ammonia (e.g. for lessening the hazards), respiratory equipment and protective clothing must be worn. A gas mask can be regarded as a limited respiratory equipment. Providing there is sufficient oxygen in the atmosphere, the gas mask fits tightly and the special ammonia filter has been screwed into the gas mask, contaminated rooms may be entered for a limited period of time, if certainty exists, that the ammonia content is below 2 %. The filter manufacturers data will give precise information on the time limit, the

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maximum permissible ammonia concentration and the life of a new gas mask filter the container seal of which has not yet been broken. A sufficient number of gas masks should be available at all points where ammonia might possibly escape to enable operating personnel to evacuate the plant quickly. If, for any reason, a gas mask should not be available, the next best protection will be afforded by holding a wet rg over nose and mouth. In emergencies, a dry handkerchief or a sleeve will afford some protection. In all such cases it is important to choose a route of escape against the wind. The breathing apparatus is used whenever the ammonia concentration exceeds the limit value mentioned above or if it is not known (or if it is likely to alter), if the oxygen content is too low, or if the life of the gas mask filter is likely not to be adequate. Breathing apparatus of the type connected by means of a hose to an air intake located in a non-contaminated area will frequently have a too high line resistance and will mechanically impede both the work and the radius of action. Better maneuverability is achieved with breathing apparatus incorporating compressed- air bottles. Any person using such breathing apparatus should, prior to use, ensure that sufficient air is contained in the bottle, the valve is set correctly, the hose connection is properly fixed, and that the mask fits properly. In addition, it is important that persons working in rooms contaminated with toxic gases are observed from the outside and that suitably equipped personnel is standing by to rescue such persons in emergencies. Over and above the respiratory equipment mentioned, personnel in hazardous areas should wear protective clothing covering the whole body. Such protective clothing comprises:

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1.A long-sleeved working jacket. 2.Long trousers and underwear, if possible, made from cotton, since cotton is more resistant to alkalis than wool. 3. Rubber boots. 4.Rubber gloves. 5.Protective helmet with rim. The sleeves should be worn outside the rubber gloves and the trousers outside the boots. Certain areas of skin can also be protected by an ointment or oil. If necessary, the above-mentioned protective clothing can be replaced by a tight anti-gas suit covering the whole body. First aid: It is of primary importance to take the injured person out of the endangered area as quickly as possible. In case of serious injuries or of any injuries to the eyes, a medical practitioner must be summoned at once. In the meantime, as much ammonia as possible must be eliminated. e.g. by dousing with plenty of water, discarding contaminated clothing including underwear. The patient should then be made to lie down and wrapped in blankets to keep him warm. Eye contact:ammonia must immediately be washed with plenty of clean

water .This can be followed by an eye bath in diluted acetic acid (0.5 %) or boric acid (3%), after which the eyes should again be washed with clean water. breathed contact:in, inhalation of steam or vinegar vapor is recommended.

Artificial respirator is forbidden .If possible, the breathing air should be enriched

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with oxygen. swallowed contact:If ammonia-bearing water has been swallowed , the

patient may be given milk to drink providing he is fully conscious.

4. Nitric acid(HNO3):
Nitric acid is a color less liquid which gradually turns ye Wow owing to decomposition phenomena under the influence of light or heat. When the acid is kept in open vessels, it will discharge vapors which generally contain nitrous gases. Nitric acid figures among the strong acids; in addition, it features marked oxidizing characteristics and will seriously attack numerous metals and organic substances. In case of contact with the human skin, it will produce burns whose seriousness depends on the concentration of the acid. The affected zones of the skin assume a yellow color . Large-area acid burns the skin might be lethal, serious injury of the eyes might lead to a loss of the eyesight. When drinking nitric acid, mucous membranes will suffer burns that might be lethal.

Protective measures: Persons working on piping or vessels containing nitric acid must wear protective goggles. Better safety is achieved through the use of protective globes of transparent plastics that cover head and neck. Hands can be protected through rubber gloves which, however, have only a limited resistance to concentrated acid .Suits of felt or special plastics are adequate for use as protective clothing. It is imperative to wear a gas mask when working in any area where nitrous gases

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or nitric acid vapors might be encountered. Respiratory equipment should be used even when a slight increase in nitrous gas concentration is detected because normal filter elements might break down. Concerning the maximum permissible nitrous gas concentration, the specifications furnished by the manufacturers of gas mask filters shall be observed. Spilled acid shall not be taken up with the aid of cloths, sawdust, clean or oil-bearing cleaning waste. For removing the acid, it might be advisable to neutralized with lime or soda ash (pay attention, however, to the evolution of CO2) and flush the whole into the sewer with large quantities of water. First-aid measures: Skin contact:After contact of nitric acid with the skin, flush immediately

with large quantities of running water and subsequently with a dilute sodium carbonate solution (5 to 7 % concentration). Clothing soaked with nitric acid shall be removed immediately. For large-area burns it is recommended to flush the skin under a shower or with the aid of water hoses and water-filled bath tubs. The personnel must be clearly aware of the location where flushing facilities are installed. To avoid sub cooling of the body, it is recommended to use lukewarm water if flushing must be continued for any appreciable time. No oil, ointment, tar or flour shall be administered to acid burns on the skin. Any person who has suffered acid burns shall consult a physician. Eye contact:Immediate and intense flushing with large quantities of water

shall also be done in the case of acid burns in the eyes. The eye lids shall be held apart to ensure full exposure to the flushing water. Immediate subsequent medical aid is imperative. Swallowed contact:If nitric acid has penetrated into the mouth of a person,

the patient should immediately be allowed to drink large quantities of lukewarm

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water to dilute the acid swallowed. Early medical aid is absolutely necessary. A stomach tube shall be administered by a physician only, because any organs that have suffered acid burns are easily bound to be injured.

5. Nitrous gases:
The oxidation of ammonia, the reaction of nitric acid with reducing substances, and the decomposition of nitrate-bearing substances are accompanied by the formation of the extremely poisonous nitrous gases which are a mixture of various oxides of nitrogen .Nitrous gases are a very malicious poison because the immediate nuisance after inhaling is negligible and the seriousness of the poisoning does not appear before expiration of several hours. Few breaths in a fairly poisoned atmosphere might be sufficient to destroy the tissue of the lungs to a point where a lethal edema of the lungs might occur even 8 hours or more after exposure, unless adequate aid is administered in good time. The symptoms of serious affection, such as headaches, fatigue, low blood pressure, will sometimes commence after several hours only. Subsequent effects are the bluing of the lips, shallow breathing, death from suffocation. It is absolutely imperative that any person who has inhaled nitrous gases consults a physician even if no signs of indisposition are apparent. The maximum permissible concentration of oxides of nitrogen at the working place is about 9 mg/m3 (5ppm). A short-time exposure to an atmosphere containing 25ppm N02 might be injurious to health; a lethal effect must be expected at 200 ppm. Protective measures:

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In case of an eruption of nitrous gases, the personnel shall leave the- place of eruption as quickly as possible and in a direction opposite to the wind direction. Actions to be taken for eliminating the evolution of oxides of nitrogen depend on the cause of such evolution. Personnel shall approach the point of leakage from a direction which is opposite to the wind direction. As mentioned before, the protective effect of gas masks is limited by the gas concentration and the time of exposure. For further details, reference should be made to the specifications furnished by the manufacturers of the gas masks. Better safety is achieved with respiratory equipment. The use of suitable gas protective clothing is also recommended. First-aid measures: Any person who has inhaled nitrous gases should immediately be removed to fresh air and should be covered with blankets and kept quiet until the physician arrives. The patient shall not move even if he feels able to do so. It is recommended to enrich the breathing air with oxygen and to allow the patient to inhale the fumes of an ammonium bicarbonate solution. Artificial respiration should not be administered. The use of oxygen should be done very centious and only in the presence of a physician having special education in this field. If no physician is available at short notice, the patient should be taken on a stretcher to the nearest hospital.

6. Oil/amine solution:
Oil/amine solution is a chemical product which by repeated or prolonged contact with skin may cause irritation or health hazards. By contact with the eyes damages to the eyes may occur. Flammable material .

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Protective measures: Contact with eyes, inhalation of spray mist, skin contact directly or by using of clothes, shoes etc. contaminated with the product, should be avoided. Protective goggles, plastic gloves and proper clothes should be used during work in the oil/amine section of the plant. First-aid measures: Spillage:Fire:Absorb in earth or sand and remove to safety place. Extinguish with carbon dioxide or powder. Wipe of the product wash with water and soap. Wash with a

Skin contact:-

solution of 3 % acetic acid in water. Rinse carefully with water. Get medical attention if symptoms arise. Eye contact:Immediately wash with 0.5 %acetic acid in water, then give a

prolonged (15-20 mm.) irrigation with water. Get medical attention. Ingestion:Do not induce vomiting.

7. Granulating aid:
This description is based on granulating aid of Galoryl-type. For other agents, which can be used in the plant, manufacturer instructions should be observed. Granulating aid is a anionic surfactant of sulphonate type, total soluble in water. Contact with eyes, inhalation of spray mist, skin contact directly or by using of clothes contaminated with the product should be avoided. Protective measures: Protective goggles, plastic gloves and proper clothes should be used during work with granulating aid.
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First-aid measures: Spillage:Wash down area with water Waste disposal method: Biodegradability 91 PCT. Comply with ocal regulation concerning industrial surfactants (detergents) Skin and eye contact:flush immediately with plenty of water, avoid contact with skin and mucous membranes Ingestion: Do not induce vomiting as for household detergents. Consult a physician.

8. Protective equipment:
In order to prevent accidents and to lessen their effect, suitable clothing should be worn covering the whole body other than head and hands and, in addition, the following items of protective clothing and respiratory. equipment should be readily available: 1.Protective helmets. 2.Goggles and acid-proof hoods 3.Gloves, partly of rubber, wool and leather 4. Rubber boots 5. Rubber protective suits 6. Gas masks with appropriate filters 7. Breathing apparatus 8. Tight anti-gas suits 9.Shower-baths for washing oft corrosive substances
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10. Sodium carbonate solution (5-7 %) for post treatment after acid burns on skin 11. Eye-bath flasks with clean water 12.Eye-bath flasks with 0.5 % acetic acid or 3 o,/ boric acid 13. Stretchers with blankets 14. Instructions on the first aid to be given in case of accidents, poisoning and burns caused by the chemicals used in the plant. It is extremely important to check continuously the protective equipment and to maintain it in a fully serviceable condition at all times.

8.1 General measures to reduce the danger of accidents: Accidents can be avoided if:
The production plant is always kept clean and in technically proper condition. Any cotton rags, paper, other waste, tools, instruments no longer used, and similar, must be kept in special containers or at special places. Escape ways and fire escapes must be kept free. Absorption towers must only be mounted if a serviceable gas mask is carried along. Protective covers on mobile parts of the equipment must be orderly fixed. Cleaning works on running machines should not be made.

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 Stays under pending loads should be avoided. For works which cannot be carried out from firm platforms skeletons must be expertly erected, or if possible, steps as prescribed by directions can be used. In case of open erection holes, handrails must be provided. For works in some height safety belts must be worn. A protective helmet should always be worn in the production plant. Entering of the production plants is not admitted to unauthorized persons. All persons not concerned with the operation of the plant, must leave the plant. All necessary repairs must be carried out at once, and only by the competent personnel after contacting the shift foreman and previous checking of the respective aggregate. To avoid misunderstandings the order is best given in writing and completion of the work is also confirmed. Hints about suitable protective measures, marked on this order, can be very useful. This applies especially for welding works and the use of open flames in the production plant. When using solvents, the appropriate instructions to avoid explosive ratios or health injuries must be followed. The personnel must be informed of the safety regulations and accident instructions at regular intervals.

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8.1.1 Special measures to prevent accidents when working on electrically driven equipment and machinery: When working on electrically driven equipment and machinery the shift foreman must order, via the competent electrician, the shutoff resp. the protection against unallowable switching in. This comprises proper switching off, taking out of fuses, resp. locking of switches with safety locks or disconnecting of the cutoff knifes. At the appertaining switch a sign Switching on prohibited must be hung up. Only after having taken these measures the shift foreman may allow the repair. After completion of repair works the shift foreman must convince himself of the correctness and determine whether the equipment can be switched on again without danger. If there is no danger, he has the machine tripped again by the operating electrician. During this procedure the shift foreman must be present. 8.1.1.1 Special measures to prevent accidents during sampling: Sampling is done by specially trained personnel. The person taking samples must wear protective equipment as goggles, gas masks etc., which corresponds to the special situation and material. The sample must be filled only into the special sampling container. Special care must be taken when the agent is on pressure or has a very high resp. very low temperature. If the sampling valve is not movable, great power strains should be avoided. It must be brought into proper operating condition in due time. Transport of the sample must be made with the necessary care. Dangerous materials must be protected against splashing, e.g. when stumbling on stairs etc., and should be put into containers which can be locked.

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8.1.1.2 Special measures to prevent accidents while opening and inspecting vessels and equipment: Opening of vessels and equipment. Before opening vessels and equipment, these must be drained as far as this is required for safety reasons. If the vessel was under pressure, it must be expanded effectively beforehand. When opening the vessel, the bolts of the flange connection or the lid on the remote side and opposite to wind direction have to be loosened first. Thereafter the lid or the flanges still held by some screws equally distributed on the periphery, must be slightly vented and loosened that much, that it does not stick or rest on the gasket seat. If there is no overpressure anymore, the flange connection can be fully loosened, the lock completely unscrewed or the lid taken off. If the vessel was containing toxic material before drainage, health can be endangered by the streaming out agent; or if the material showed a very high resp. 8.1.1.3 Special regulations for the inspection of vessels, equipment etc: Before inspection of a vessel etc. this must be drained first, and if possible, cleaned by flushing from outside. By interrupting the feed lines, in exceptional cases by inserting blind flanges, the feed of any endangering materials must be eliminated. If toxic or narcotic gases can collect in the vessel or equipment, the personnel can only inspect this when wearing proper gas masks. If inflammable gases or explosive gas mixtures can form up in the vessel, a good venting must be carried out to remain below the ignition limit. When using electric lamps and instruments in vessels of good conducting materials, protective measures against contact potential become necessary. Portable lamps must only be used up to low voltage of 42 V. The electric instruments and their supply lines must be checked for their irreproachable condition before use. It must be secured, that the electric

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supply lines cannot be damaged during work. Before inspection of vessels or equipment which are movable or have movable internals, i.e. drying drums, centrifuges, tube vessels, bucket elevators, etc. measures must be taken against unallowable and unintentional starting or moving. For this purpose the electric drive can be switched off by disconnecting all conductors, by locking the switch or by interrupting the corresponding electric fuses. An unintentional moving of the internal parts can for instance be avoided by arresting the brakes of the drive or by blocking the movable parts. The person entering the vessel must be tied to a safety belt and watched by somebody outside. This person must not leave, and in case of need further assisting persons must be made available. Any persons also entering the vessel must be equipped correspondingly, in case of need also the watching person. After completion of the work the vessel must only be brought into normal operating condition, after the supervisor has convinced himself, that the personnel has left the equipment and that order was given to the personnel, not to enter the vessel or equipment again. 8.1.1.4 Special measures to prevent accidents during welding works: Rooms where welding works are to be carried out, should be vented correspondingly. Small rooms or vessels must be constantly vented with fresh air, or the personnel must use oxygen equipment. Before starting work it must be made sure that no danger of fire or explosion exists. When working on containers and vessels, these must be opened and cleaned beforehand. When working on hollow bodies the formation of a dangerous overpressure must be avoided. During welding works in the neighborhood of inflammable building parts, i.e. wood or similar, safety precautions must be met to avoid fires, e.g. by covering all inflammable parts, disposal of extinguishing water or other suitable fire extinguishing instruments. The heated spot or the endangered neighborhood must be watched until there is no longer a noticeable over-temperature.

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9. Fire protection devices:

The operating personnel must be made familiar with the fire protection and fire extinguishing equipment. The fire extinguishing equipment should be easily accessible and clearly marked. A use for other purposes should be prohibited. In case of fires to the aggregates which are under electric voltage, the use of foam extinguishers or the spraying with water should be waived due to the connected danger of accident (electric shock). In this case carbon dioxide or dry extinguishers are suited for use. Carbon dioxide- and foam extinguishers can also be used in case of oil fire. Fire extinguishers containing tetrachlorine dioxide, often develop toxic gases. For this reason use of these instruments is appropriately waived. If the fire stretches over to ammonium nitrate containing fertilizers or nitric acid tanks, it is recommended to use water, if this is not prohibited due to special circumstances.

CAUTION: When approaching any fire in the granulation plant, always have self- contained breathing apparatus immediately available. Fumes from the decomposition or the burning of ammonium nitrate are extremely toxic.

9.1 Fire fighting:

For localized fires in motors, gears, conveyors, etc. (not involving ammonium nitrate) take the following actions: Shutdown the affected equipment. If the affected equipment is connected into the granulating plant interlock

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system, also shutdown coating drum and transport conveyor to storage. Notify the plant fire station of the location and nature of the fire. Then, use portable CO2-type fire extinguishers on the fire. If equipment containing solid AN is exposed to the flames or to excessive heat from the fire, apply water with a hose to the solid AN immediately. Use as much water as possible. While the clean-up job after the fire will be increased .

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CHAPTER 8 TROUBLE SHOOTING

1. General aspects. 2. Neutralization troubles. 3. Granulation troubles.

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1. General:
This section describes trouble situations that may occur in the neutralization and granulation plant, their most likely causes and the pertaining corrective actions. Those operation disturbance are the expected teething troubles of a new plant that airse more from equipment malfunction than from inherent process malfunction. The following description focuses on the granulator and on its feed only. Mechanical troubles - limited in number as the equipment is fairly sturdy and simple - are left aside.

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2. Neutralization troubles:
UPSETS CAUSES ACTIONS (SEQUENTIAL) Control level in the HNO3 tank and the 1. Low level is Control valve of nitric acid is more open then in normal case Ncontent in the processInform the personal of 1. To high water content in the NH3evaporation system 2. Upset operation of the evaporation the NH3 evaporation unit. Reduce plant load nitric acid tank 2. Pump failure HNO3-pump function Start up spare pump if necessary. Reduce plant load

1. Low pressure of nitric acid.

2. Low pressure of NH3-gas control valve for NH3-flow open more then in normal case.

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1. Load of the plant too high/low 3. AN-solution temperature outlet reactor 43R001 too high/low 2. Vapor pressure in 31 C00l is too high 3. Injection water quantity is too low/high Reduce/increase plant load Reduce/increase pressure in 31 Cool (PIRCA 43025) Increase/reduce injection water quantity Check the concentration

UPSETS

CAUSES

ACTIONS (SEQUENTIAL Decrease the temperature Decrease

4. Concentration in tank 31 T00l is high

1. Water evaporation during a longer shutdown of the plant

the concentration by adding of water. Check pHvalue and adjust if necessary

1.low vacuum in C001 5. the tempTI011/111 of the reactor R001 is high 2.high concentration of HNO3 to the reactor

Check pH-value and adjust if necessary Opened FIC414/464 Check for PIC213/313

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6. The temp TI011/111 of the reactor R001 is low 1. Low concentration of HNO3 is Low

7. Concentration in tank 31 T00l is Low and temp also

1. the condensate line to 31 T001 have leakage throw in XV valve

Close manual valve before and after XV valve

8.2 Granulation troubles:

UPSETS

CAUSES

ACTIONS (SEQUENTIAL)

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1.Flushing air for level pressure probe deviates. 2.Granule size too small (also high recycle rate. 1. Granulator Bed Level Rises 3.Choking of the passage by: a. dissimilar level in respective chambers b. flapper valve restricts flow. c. clogged perforated plate. 1. Unstable granule 2. Bed Level Oscillation size. 2. Unstable level control valve. 1.To adapt crusher/sieve adjustment. 2. Tuning of control valve to be optimized. ACTIONS (SEQUENTIAL 2. See Product in Granulator too fine 3a. Stop injection, control passage under flow weir. 3b. See related to granulator discharge. 3c. Stop injection, empty granulator out, check and clean perforated plate. 1.Cleaning of flushing tubes and reset of identical air flow rate through flow meters.

UPSETS

CAUSES

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3. Bed Slugging

1.Fluidization air flow 1. To reduce it. rate too high. 2. See Product in 2. Too many fines. Granulator too fine. 3. Too little size 3. Delay capacity differential between increase. subsequent chambers 4. to raise it and (specially at start-up). increase differential. 4. Too little fluidization air flow rate differential between adjacent chambers.

4. Product in Granulator too fine

1. To increase 1. Fine dust particles. fluidization air flow insufficiently entrained rate without onset of entrainment. 2. Product crushed by 2. To reduce atomization! fluidization fluidization air. atomization air flow 3.Crusher generates rate too many nuclei 3. Temporarily stop crusher feed. 1. Too much fine particle entrainment 2. Recycle of too large crushed nuclei.

5. Product from Granulator too Coarse

1. Lower fluidization air flow rate. 2. Set correct roll gap.

UPSETS

CAUSES

ACTIONS (SEQUENTIAL

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1. No additive feed. 6.Dust formation 2. Excessive spray nozzle load

1. Check additive feed. 2. To reduce AN injection.

7.Presser oscillation and solution flow rate oscillation 8.The screen of the final product not good

The basket of filter is full The size of the granules have high amount of small size

Change over 32 F002

Follow up for screen by converting 1.Check for level on 32C001.

9.The open of 32K001is big

The spraying on venturi-element not enough

2.check for discharge presser of 32 P003. 3.check for open of 32K004.

10. Moisture Content and Product too high

1. AN flow rate too high. 2. AN concentration too low. 3. Too low bed temperature. 4. Bed level too low. 5. Moisture absorption in cooler.

1. To reduce it. 2. To check. 3. To increase it. 4. Check moisture/rain entrainment in cooler air feed.

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