Operating Manual NPK Phonska II

Client: PT PETROKIMIA GRESIK
OPERATING MANUAL Plant: R&F OPERATION PF-1 PLANT

Location: GRESIK- E.JAVA-INDONESIA
Date: MARCH-03 Page 1 of 205
FOREWORD
The purpose of this OPERATING MANUAL is to provide operators with basic information
and operating instructions required for the correct and safe operation for DAP/NPK plant
of the PF-1 (TSP) Plant located in Gresik.
As experience is gained with the Plant, operating conditions and procedures may be
varied, within the safe operating limits of the equipment, to obtain optimum performance.
This manual includes sections describing the process, process control systems, start-up
and operation procedures and hazards and safety practices associated with the Unit.
The Engineering Design Book and the manuals supplied by the equipment manufacturers
supplement and complete the information given in this Operating Manual. Consequently,
operating personnel should be familiar those sources of detailed information as well.
The flows and control points given in this instructions are calculated for design conditions
only, and do not imply warranted performances.
INDEX
CHAPTER 1 - GENERALITIES
1.1 Introduction
1.2 Basic characteristics of the process
1.3 Design basis
CHAPTER 2 - PLANT DESCRIPTION

2.1 General description of the unit
2.2 Main characteristics of the plant design and operation
2.3 Interlocking system
CHAPTER 3 - PREPARATION OF THE PLANT

3.1 Initial plant preparation and check
3.2 Daily data log sheet
CHAPTER 4 - GENERAL CONTROLS OF THE PLANT

4.1 Analytical methods and sampling
4.2 Checking and cleaning procedures
CHAPTER 5 - PLANT SAFETY

5.1 Introduction
5.2 Ammonia
5.3 Phosphoric and sulphuric acids
5.4 Safety during maintenance
5.5 Restricted access areas
CHAPTER 6 - DAP and NPK MANUFACTURE

6.1 Plant capacity
6.2 Product specifications
6.3 Raw materials and utilities consumption
6.4 Process
6.5 Plant start-up operations
6.6 Normal plant operation. Potential operative problems.
6.7 Plant shut-down procedure
6.8 Change in product manufacture
CHAPTER 7 - PHYSICAL AND CHEMICAL DATA
CHAPTER 8 - MASS AND ENERGY BALANCES

8.1 Mass and Energy balance for DAP 18-46-00
8.2 Mass and Energy balance for NPK 15-15-15
CHAPTER 9 - DIAGRAMS
9.1 Process Flow Diagrams
9.2 Piping & Instrumentation Diagrams
9.3 Interlock Diagram
CHAPTER 1 - GENERALITIES
INDEX
1.1 INTRODUCTION
1.2 BASIC CHARACTERISTICS OF THE PROCESS
1.3 DESIGN BASIS
1.3.1 Climatic conditions
1.3.2 Raw material specification (At battery limit)
1.3.3 Utilities specification
1.3.4 Plant product specification (Main products)
1.3.5 Production capacity
1.3.6 Plant effluents
1.3.7 Raw materials & utilities consumption (per Ton of product)
1.3.8 Input/output table at battery limit

1 GENERALITIES
1.1 INTRODUCTION
This operating manual applies to the revamped TSP-1 plant to produce DAP/NPK
granular fertilizer (maintaining TSP production) by PT Petrokimia Gresik in Gresik
E.Java (INDONESIA), according to the project developed by its Detail Engineering
Department on the basis of INCRO, S.A. technology.
This operating manual refers more specifically to the production of DAP and several
grades of NP/NPK, specially 15-15-15 via sulphuric acid. Other products could be
produced following chapter 2.6 production capacity of Basic engineering document
where are shown different grades such as 23.10.10, MAP, 16.20.0.
Fertilizer Plant has been built according to INCRO, S.A. technology, which uses its
own designed Pipe Reactor (PR) and conventional Preneutralizer (PN). The same
type of PR is being used in many other fertilizer production units around the world
(Brazil, United Kingdom, Turkey, Tunisia, Japan, Taiwan, Portugal, Saudi Arabia,
Korea, India, China... as well as Spain) since more than twenty five years ago.
Some of those units are also using mixed process. New plant includes singular
INCROs PN design and in this case essential modifications have been included to
achieve optimum performance of existing one.
The information contained in this operating manual will be the basic guide to follow
in the manufacture of the above mentioned products, without prejudice to any
possible adjustments in the parameters and/or operating instructions that the
operative practice of the unit may advise.
1.2 BASIC CHARACTERISTICS OF THE PROCESS

The process to be followed in the manufacture of the products referred to in this
operating manual is based on the mixed process Pipe Reactor + Preneutralizer
(PR+PN) which consist on the use of a Pipe Reactor (PR) of small dimensions,
developed by INCRO S.A., and a conventional Preneutralizer (PN), for the
neutralization of phosphoric acid and/or sulphuric acid with ammonia.
DAP, 18-46-0, will be normally produced using the above PR+PN mixed process,
but it will be also possible to produce this grade only from PR process by using two
provided Pipe Reactors A/B in parallel.
For sulphuric acid based (SAB) NP/NPKs production, like when manufacturing
15.15.15, 20-20-0, 16.20.0 using exclusively ammonia as N source, the necessary
ammonium sulphate slurry will be made in the existing preneutralizer and the
ammonium phosphate slurry required quantity will be split between PR and
preneutralizer.
To produce urea based NPK grades like 23.10.10, 15.15.15, 20.10.10, the
process to be used will be similar to the one presently employed in PHONSKA plant,
with all the slurry being produced in the PR.
In all cases the remaining ammonia is introduced through an ammonisation

ploughshares system of high efficiency, developed by INCRO, S.A., which injects
the ammonia deep in the granulator solids bed.
The use of the INCRO, S.A. Pipe Reactor jointly with the optimized Preneutralizer
gives a great flexibility to the system, making it easily adjustable to the type of
production required.
1.3 DESIGN BASIS

1.3.1 Climatic conditions
Ambient temperature
Dry bulb temperature
- Summer: 36C maximum, 33C for design
- Winter: 22C, minimum
- Average 33C
Wet bulb temperature
- Mean humidity, night (23 C) 96%
- Mean humidity, day (33 C) 70%
Barometric pressure
1033 mbar. At sea level
Rain fall
Maximum for 15 minutes: 120 mm
Maximum for 1 hour: 80 mm
Rainy seasons: From December to April
Wind
Prevailing direction: WNW November to April
ESE from MAY to October
Maximum wind velocity 40 km/h. Exceptionally 120 km/h
Earthquake
Code Parasismic: 0.3
Zone Point of Mercalli scale
Site elevation
At sea level
Others
Thunder and lightening to be considered.
1.3.2 Raw material specification (At battery limit)

a) Ammonia
State Liquid
NH3 content 99.5% w/w min
H2O content 0.5 % w/w max
Oil content 0.1 ppm
Pressure at B.L. 12 kg/cm2 (min + 3 kg over
equilibrium pressure)
Temperature -33 C
b) Phosphoric acid
P2O5 48 -50% minimum

Solids 3-4 % maximum
SO42- 2.5 % maximum
Specific Gravity 1.650-1720
Temperature 33 C
Pressure 4 kg/cm2 min
c) Sulphuric acid
H2SO4 content 98 % typical

Pressure 4-5 kg/cm2
d) Ammonium sulphate
Nitrogen 21 % min.
H2SO4 0.1 % max.
Moisture: 1 % max.
Size USA stand. mesh 30
(600?m) 75%
Free flowing, <100 ppm as organic matter
e) Urea
Nitrogen 46% minimum

Moisture 0.5% max.
Size USA stand. meshes 18-6
(1-3.35 mm) 97%
Free flowing
f) Potassium chloride
K2O 60% min.

Moisture 1% max.
(150?m 1.18 mm) 95%
Free flowing <100 ppm, as organic matter
g) Kieserite
MgO 27% min.
Moisture 1 % max.
(1mm 3.35 mm) 90%
Free flowing
h) Filler
Type Sand, clay

Moisture 10% wt max
Granulometry USA stand. meshes 100-30
(150?m 600?m) 90%
Free flowing
1.3.3 Utilities specification
a) Steam
Low pressure Saturated, 7 kg/cm2, for flushing
b) Process / service water
Pressure 3 kg/cm2
Temperature Ambient
pH 7.5 8.5
c) Instrument air
Pressure 7 kg/cm2
Temperature Ambient
Dew Point - 10 C
Oil free
d) Plant air
Pressure 7 kg/cm2 min.
Temperature Ambient
e) Fuel
Type: Natural Gas
Calorific value: 10800 kcal/kg
f) Power
- Frequency 50 Hz
- Large Motor (over 150 kW) 6000 V, 3 phases
- Small Motor (up to 150 kW) 380 V, 3 phases
- Lighting 220 V
- Instrument 110 V
- Control 24 V DC
g) Defoamer
Oleic acid or similar
h) Coating agent
It is composed of:
- One solid, like tack, caolin kieselgur, celite
- One oil (SK INCRO CO-98, Mobil) aminated.
1.3.4 Plant product specification (Main products)
NPK 23.10.10 15.15.15 DAP MAP OTHER NPK

Total N (%) 23 + 0.9 15 + 0.9 18 ? 0.5 11 ? 0.5 ? 0.5
Total P2O5 (%) 10 + 0.9 15 + 0.9 46 ? 0.5 52 ? 0.5 ? 0.5
W.S. P 2O 5 (%) 8 + 0.9 13 + 0.9 40 ? 0.5 45 ? 0.5 ? 0.5
K2O (%) 10 + 0.9 15 + 0.9
Moisture (% max) 1-1.5 1-1.5 1-1.5 1-1.5 1-1.5
Particle size:
(1-4 mm, % min) 90 90 90 90 90
(2-4 mm, % min) 85 80 85 85 80-85
Hardness:
(kg/cm 2 min) 1.5 2.5 3.0 2.5 1.5-3
1.3.5 Production capacity
Product Dry Min Throughput (t/h) Production (t/h)

time recycle
(min) (min) Dryer Plant Guaranteed Expected
23.10.10 20 212 241 318 1140 1191.3
15.15.15 14 307 344 350 1520 1567.5
DAP 12.5 314 374 375 1250 1300
20.10.10 20 212 241 318 1140 1187.5
MAP 14 245 250 350 1615 1710
13.13.17.2 14 307 344 350 1520 1567.5
Other NPKs 12.5-20 212-314 241-374 318-375 1140-1615 1187.5-2000

15.15.15 (H2SO4) 12.5 314 374 375 1320 1375
16.20.0 (H2SO4) 12.5 314 374 375 1400 1450
1.3.6 Plant effluents
Gaseous Exhaust Stack Vent Analysis

Ammonia 40 mg/Am 3 max
Dust 50 mg/Am 3 max
HF 5 mg/Am 3 max
1.3.7 Raw materials & utilities consumption (per Ton of product)
The following consumptions of raw materials are guaranteed in kg by ton of product.

The first value applies for the raw materials in final product plus stack losses,
whereas the second includes consumption through feeders / meters and therefore
its accuracy.
Items 23-10-10 23-10-10 15-15-15 15-15-15 (H2SO4) DAP (alt. 1)

Ammonia 59-62 59-62 82-85 175-180 222-226
Urea 262-265 402-406 36-38 15-16 0
Amm.Sulphate 307-308 0 328-331 0 0
P2O5 (100%) 103-104 103-104 153-154 153-154 464-469
Sulphuric acid 50 50 60 316-320 30
KCl 169-171 169-171 252-255 252-255 0
Filler 0 164 0 0 30
Kieserite 0 0 0 0 0
Electrical kWh 62.7-67 62-67 52-56 64-69 64-69
Water, m 3 0.1-0.15 0.1-0.15 0.15-0.2 0.4-0.5 0.3-0.35
Steam, (t) 25-29 25-29 20-27 60-65 40-48
Natural gas (kg) 6.5-7 6-7 8-8.5 4.5-6 7-7.5
Production of sulfuric acid based's NPK consumes natural gas
less than ZA based's NPK because more heat produced by neutralization
reaction between acid and ammonia so that is helping in drying process.
Items DAP (alt.2) 20-10-10 MAP 13-13-17-2

Ammonia 202-207 60-62 136-139 72-75
Urea 0 333-337 0 36-37
Amm.Sulphate 74 0 0 271
P2O5 (100%) 464-469 103-104 525-530 133-134
Sulphuric acid 0 51 0 51
KCl 0 169-171 0 286-289
Filler 0 233 46 0
Kieserite 0 0 0 80-81
Electrical kWh 64-69 62-67 47-51 88-89
Water, m 3 0.3-0.35 0.1-0.15 0.3-0.37 0.13-0.17
Steam, (t) 40-48 25-29 26-31 20-27
Natural gas l (kg) 7-7.5 6.5-7 7-7.5 8-8.5
1.3.8 Input/output table at battery limit
Pressure Temp. C Quantity (3)

TSP1 TSP1+2
Input
Phosacid 50% P2O5 4 kg/cm 2 Amb. 50 67 MT/h 120 MT/h
Sulphuric acid 4 kg/cm 2 Ambient 30 MT/h (4) 60 MT/h (4)

(20m 3/h) (40m 3/h)
Liquid ammonia (1) 12 kg/cm 2 -33 15 MT/h 30 MT/h
Filler Grav. Ambient 15 T/h 30 T/h
Urea Grav. Ambient 30 T/h 60 T/h
Potash Grav. Ambient 30 T/h 60 T/h
Ammonium sulphate Grav. Ambient 35 T/h 70 T/h
Kieserite Grav. Ambient 10 T/h 20 T/h
Defoamer (barrels) Ambient 0.2 m 3/h 0.4 m 3/h
Process water 3 kg/cm 2 Ambient 25 m 3/h 50 m 3/h
MP Steam (sat) 7 kg/cm 2 (2) 164 2500 kg/h 4000 kg/h
Fuel Oil / PG Ambient 150-800 kg/h1200 kg/h
Output
Final product Grav. 55 92 t/h
(1)
Always 3kg/cm 2 over equilibrium pressure. tekanan minimal 3 kg/cm2 di atas tekanan kesetimbangan
(2)
Minimum required specification.
(3)
For each train.
(4)
30 MT/h are required to produce grades like 16-20-0, 16-16- 8, 20-20-0 with high quantities of
H2SO4.
CHAPTER 2.- PLANT DESCRIPTION

INDEX
2 PLANT DESCRIPTION
2.1 GENERAL DESCRIPTION OF THE UNIT

2.1.1 Introduction
2.1.2 Description of the equipment
2.2 MAIN CHARACTERISTICS OF THE PLANT DESIGN AND OPERATION

2.2.1 Ammonia feeding
2.2.2 Phosphoric and sulphuric acid feeding
2.2.3 Main reactions
2.2.3.1 Preneutralizer
2.2.3.2 Pipe Reactor
2.2.4 Granulation
2.2.5 Drying
2.2.6 Screening and grinding
2.2.7 Product extraction and cooling
2.2.8 Polishing screening and conditioning
2.2.9 Main Fans
2.2.9.1 Granulator exhaust fan
2.2.9.2 Dryer exhaust fan
2.2.9.3 Rotary cooler fan
2.2.9.4 Cooler and dedusting exhaust fan
2.2.10 Dust collection and recovery. Air preheating to dedusting system
2.2.11 Scrubbing system
2.2.11.1 General
2.2.11.2 Scrubbing system units
2.2.11.3 Scrubbing system control
2.2.12 Pipe Reactor vessel feedings
2.2.13 Liquids drainages
2.2.14 Solid raw materials dosage
2.3 INTERLOCKING SYSTEM

2.3.1 Interlocking sequences
2 PLANT DESCRIPTION
2.1 GENERAL DESCRIPTION OF THE UNIT
2.1.1 Introduction
The unit consists of two TSP granulation trains, one of them being presently
revamped to produce DAP and various NPK grades, using ammonia, urea,
ammonium sulphate, phosphoric acid, sulphuric acid, potash and filler as main raw
materials.
The unit is designed to produce the following grades with the following production
capacities :
Product Production (t/h)

Guaranteed Expected
23.10.10 1140 1191.3
15.15.15 1520 1567.5
DAP 1250 1300
20.10.10 1140 1187.5
MAP 1615 1710
13.13.17.2 1520 1567.5
Other NPKs 1140-1615 1187.5-2000
15.15.15 (H2SO4) 1320 1375

16.20.0 (H2SO4) 1400 1450
They will be produced with the granulation process developed and licensed by
INCRO S.A., which is based on the use of a INCRO S.A. designed Pipe Reactor
installed into the granulator and the existing preneutralizer for the neutralisation of
the phosphoric acid and sulphuric acid with ammonia. For DAP production and upon
average conditions, the PR will produce between 40-50% of the total ammonium
phosphate slurry needed. The remaining 60-50% will be produced in the
preneutralizer (PN), being pumped to the granulator drum. Occasionally, if required,
full DAP slurry production can be attained with only PR, although the plant total
output will be slightly lower (around 10%).
For sulphuric acid based (SAB) NP/NPKs production, like when manufacturing
15.15.15, using exclusively ammonia as N source, the necessary ammonium
sulphate slurry will be made in the existing preneutralizer and the ammonium
phosphate slurry required quantity will be split between PR and preneutralizer.
To produce urea based NPK grades like 23.10.10, 20.10.10, the process to be
used will produce all the slurry in PR.
2.1.2 Description of the equipment
Reference is made to the process flow diagrams numbers: P-05-12-300-001 and P-

05-12-300-002, for the solid and liquid sections respectively.
Raw materials dosing
In the existing Train 1 solid raw materials transfer from their storage to the
respective bin is accomplished by several belt conveyors and solid raw material
elevator. These feeding way to equipment are not been modified by this project.
The existing raw material bins (12-BB-314/316/318A/318B/319) are slightly modified

to incorporate new discharge isolating gates and 5 big blasters (12-BB-
314/316/318A/318B/319). There are five bins to feed all required solid raw materials
to the process (Ammonium sulphate, potash, TSP-ammonium sulphate, filler and
urea).
As per considered in P&Id P-06-12-300-001 a load cell will be used as indication of

normal level in bins. Rod type level indicator is installed to indicate very high level in
bins.
In the cases, those considered levels are not already installed, other possibilities for
measuring the weigh in bins can be considered:
Ig. Installation of three vibrating rod type indicator along the wall of the bin.
First one close to the bottom as very low level indication, second one in
the middle of the bin as per normal level indicator and third one on the top
as per very high level indicator.
Optionally those level should be interlocked (very high and very low levels) with the
raw materials feeding and connected to the loading area.
In case of installing both type of weigher (load and vibrating rod) those
alarms/measure indication will also cover an eventual malfunction of the weighing
cells or a misreading in case of a very large product arching inside the bin.
At the bottom of each bin there will be a new manual bin gate (12-SR-
314/316/318A/318B/319) to isolate the respective bins, if required.
Under each of these bins there is a new wider belt conveyor feeder (12-G-
314/316/318A/318B/319), speed controlled to regulate automatically the solid
feeding rate. Feeders are mounted on loading cells (12-WQ-
314/316/318A/318B/319), which provide an indication of the real amount of flow of
material. The electronic weigher automatically measures and adjusts fed quantities
from Control Room (DCS).
Solid materials from different feeders will be discharged on the new recycle belt
conveyor (12-M-367), that also receives the recycled product from recycle drag
conveyor (02-M-304). This new conveyor will discharge on the recycle elevator (02-
M-305), whose transportation capacity has been enlarged by increasing its
operating speed.
Incros design have considered to install Urea bin and feeder as close as possible to
the end of new recycle belt conveyor (close to granulator elevator) to avoid, as
much as possible, the possible problems that could appears because of the natural
higroscopicity of the same.
A filter, usually bag type, will be also provided on top of each bin, to avoid dust
emission.
In New recycle belt conveyor, just before the feeding of raw materials, a weigher
(12-WQ-327- Recycle conveyor weigher) will be installed to measure the recycle
from the plant that it is going back to granulator.
Granulation
Discharged product from recycle elevator 02-M-305 will directly flow by gravity to the
granulator drum 02-M-361, where the granulation will take place.
Granulation is mainly accomplished by a series of chemical and physical reactions

between the different raw materials and slurries.
The P2O5 of the formulation always comes from the phosphoric acid fed to the unit.
This acid is partially neutralised with ammonia to a molar ratio N/P of 1.2-1.5,
depending on the grade, in the first reaction step. This are the most usual range for
the N/P molar ratio in that first step, but the range can be extended to 1.0-1.8 in
some cases and according the granulation process needs. For SAB (15-15-15) this
first reaction can take place with a molar ratio of 0.8-0.9 (in PN).
This first step of phosacid neutralization reaction takes place in the Preneutralizer
02-R-303 and in the Pipe Reactors 12-R-301A/B, last ones are installed so that the
slurry of ammonium phosphate is poured directly onto the solids bed of the
granulator 02-M-361. The slurry produced in the Preneutralizer is pumped by 02-P-

301A/B pumps and also poured onto the solids bed of the granulator. In case of
using only PR process, the Preneutralizer remains stopped and all ammonium
phosphate slurry is produced in one or two Pipe Reactors.
Main part of sulphuric acid, when producing NP grades (15-15-15) without urea and
high sulphuric acid content, is also partially neutralized with ammonia, together with
phosphoric acid, to a molar ratio N/S of 1.7-1.9, depending on the slurry solubility
and fluidity. This neutralization reaction takes place in the Preneutralizer 02-R-303
(N/P=0,8-0,9) and the slurry of ammonium sulphate/phosphate is pumped to the
granulator as explained before.
When producing grades with low sulphuric acid content, like DAP, 23-10-10,15-
15,15 (via ammonium sulphate) 20-10-10 etc., sulphuric acid neutralization is
partially completed in the used Reactor, according to the type of process (PN+PR or
only PR process) and in the granulator. Part of sulphuric acid can be directly fed to
granulator 02-M-361, where will be neutralized with ammonia jointly with the residual
acid content of the poured slurries.
Pipe Reactor slurries have temperatures ranging from 120 to 150C and moisture
content between 4% and 8%, although lower contents can be attained if more
concentrated phosacid is available.
Pipe Reactors have phosphoric liquor and liquid ammonia flow controls. Phosacid
liquor will be fed from Pipe Reactor Vessel 12-TK-301, by means of the pipe reactor
pumps 12-P-315A/B/C. One or two of the three pumps will be used as spare.
Co-neutralization Preneutralizer has phosphoric liquor, sulphuric acid and liquid

ammonia flow controls. Phosacid liquor will be fed from Pre-Scrubber 12-D-311A/B,
by means of Granulator Pre-scrubber pumps 12-P-312A/B. One of the two pumps
will be used as spare.
Phosphoric liquor fed to pipe reactor is made by the acid coming from the scrubbing
system, complemented sometimes by the flow of fresh phosacid fed to P.R. Vessel
12-TK-301 (not previously used into the scrubbing) plus, occasionally, some process
water, when it is temporarily required by the process..
Preneutralizer slurries have temperatures ranging from 115 to 125 C, and moisture
content between 11% and 18%, higher than PR slurries to avoid pumping problems.
Making ammonium phosphate slurry (case of ig DAP), the temperature used to
range 115-120C but making ammonium sulphate/phosphate slurry (case of 15-15-
15) this temperature increases up to 120-130 C.
Working with mixed PN+PR process, phosacid used in scrubbing system is later
splitted and sent to preneutralizer (02-R-303) and to PR Vessel (12-TK-301) in
suitable proportions.
Medium pressure steam is provided for cleaning pipe reactors. There will be an
interlocked three-position switch that will automatically shut-off feedings of acids,
ammonia and purge pot drainage On/Off valves; with a small delay, the switch will
open steam valves for flushing and recirculation lines of phosacid to PR vessel.
Opening recirculation On/off valves in PR vessel it will be avoided to damage PR

pumps (12-P-315A/B/C) meanwhile steam is fed.
MPS is also provided to clean granulator ammonia spargers.
Low-pressure steam (via installation a PSV and deheater in MPS line) is also
provided for cleaning preneutralizer and slurry pumps. The steam is connected to all
ammonia injectors and slurry pipes from the pumps 02-P-301A/B to granulator and
from the same to Preneutralizer (02-R-303). In case of any obstruction, a steam
purge is used to quickly solve the problem.
When producing TSP, LPS will be fed to granulator through existing sparger, which
must to mounted/dismounted in case of changing production from TSP (solid
granulation) to 15-15-15/DAP (slurry granulation).
To complete the acid or acids neutralization to the final required N/P ratio, up to 1.8
depending on the grade, and N/S 2.0 in all cases, an Ammoniation System Sparger
12-R-302, designed by INCRO, S.A., is provided.
The sparger is ploughshare type with arms of minimum resistance to the bed,
through which liquid ammonia is fed very deeply into the bed and distributed
lengthwise and parallel to the granulator wall, so that losses of ammonia to the
scrubber are minimized. This is a largely proven design used for more than 25 years
in all of INCRO, S.A. licensed plants.
The three items combined, PR, PN and sparger provide a great flexibility on
adjusting operation parameters in order to achieve a high efficiency.
The use of ammonia in liquid state, in the granulator, will also favour the control of
temperature into the bed, which is very important for products with a high urea
content or products with a high slurry/solid raw materials ratio in its composition.
Case of 23-10-10 and 20-10-10 or SAB 15-15-15 and 16.20.0.
No further reaction is necessary when using the INCRO, S.A. process. Therefore, all
the reactions will be completed into the granulator and product leaving it will already
have the requested levels of N, P2O5 and K2O for the product.
To make DAP, NP or NPK grades, all the necessary solid raw materials and
recirculated solids will be fed to the granulator through the recycle elevator 02-M-
305.
Recycle flow puts normally an upper limit in the production capacity of the plant.
Recycle rates will be rather low due to the low moisture content of the slurries
poured from the pipe reactor and preneutralizer.
Normally recycle ratios will be on the range 3 to 4.5 (to 1), depending on the
product. Fines, crushed oversizes and part of the commercial product, which is
returned to the granulator to keep the water and heat balance, constitute this
recycle.
Occasionally some water, coming from tail gas scrubber (12-D-312), can be directly
added to granulator to temporarily adjust granulometry, although it is not a common
and convenient practice.
Our large experience and know-how for more than 25 years, has allowed us to
establish and to develop this proposed high performance process. In many cases
products using up to 400 kg/t of prill/powdered urea as well as products with high
ammonium sulphate/phosphate slurries content, have been successfully
manufactured.
Thanks to the heat supplied by the Pipe Reactor and Preneutralizer slurries, when
urea and/or potash are present they will be very well integrated into the granules,
showing no segregation.
The granulator is provided with the possibility to vary the depth of the bed, acting on
the retaining ring plate at the solids exit side. Two emptying doors with two
possibilities for opening have been included; see granulator data sheet page 5 of 5.
The granulator will be lined with flexing rubber panels (already done), to avoid
product build-up.
Granulator is equipped with a lump kicker, see granulator data sheet page 4 of 5, to
prevent any lump from remaining inside the drum, disturbing the flow of solids and
avoiding their normal flow on the dryer. Lumps kicker will reject the lumps to an
attached grizzly, see granulator data sheet page 3 of 5, which will disintegrate them
by the rotating action.
Solids leaving granulator, normally with a moisture content around 2.0-3.0% are
gravity fed to dryer (02-M-362), in order to achieve the final requested moisture of
1.0-1.5%.
Gases developed into the granulator are sucked up jointly with the gases developed
into the preneutralizer towards the granulator pre-scrubber 12-D-311A/B, to recover
most of the evolved dust and ammonia losses.
Product drying, screening and grinding
Existing dryer will be modified in their lifting plates and rotating speed (new reducer
will be installed).
It dries solids coming from granulator to a 1.5% moisture maximum (normal 1.0-
1.5%), with a preheated air in a concurrent flow (keeping actual combustion
chamber). The gases coming from cooler cyclones will be introduced in the dryer
through new connection in the elbow of duct from combustion chamber to dryer
drum.
Existing system of air supply to dryer will be kept. No additional controls have been
added.
Dryer drum solids exit is equipped with a grizzly, to avoid any lump which could
block the screen product elevator 02-M-302. If any lump is coming out, grizzly takes
it up and throws it into a hopper which feeds the lump crusher (existing lump crusher
is out of order, it is advisable to be set it on line). Crushed lumps will join the rest of
dryer discharged product on screen product elevator.
Air leaving the dryer will contain some ammonia escaped from the product, as well
as dust carried away and water evaporated from product when drying.
This air is cycloned in the dryer cyclones 02-D-322, in order to separate the main
part of carried dust. Common hoppers are installed for each batery of cyclones, with
the corresponding discharge valve. Discharged dust joins the rest of recycled
product on the recycle drag flight 02-M-304.
After cycloning, gas will be sucked to the dryer scrubber 02-D-302. Dryer Scrubber
fan 12-C-302 is located downstream of that scrubber and it is equipped with an inlet
damper to regulate the amount of air.
A new duct tie-in in TSP reaction section is provided. A blind flange will isolate both
plants in any case, except when TSP is simultaneously produced. So reaction gases
will be scrubbed in TSP-1 plant. For adjusting flows and pressure drops a damper is
provided to control them.
Dried product is directly fed to the screen feed elevator 02-M-302, from where the
flow is splitted to two recycle drag feed conveyors (02-DR-101/102) which convey
the product to the four process screens 02-F-301A/B/C/D in the same way than
previous situation to the revamping.
New meshes will be installed in the existing screens.
The on-size product from screens passes directly to screen product conveyor (02-M-
303) and from this to Product feeder (02-D-326). This conveyor will be equipped
with a variable speed motor, controlled from the Control Room panel according the
set point of the product extractor weigher 12-WQ-326, to regulate the amount of
commercial product to the final treatment section. Subsequently, the on-size product
not sent to this section falls to the recycle drag conveyor 02-M-304, by overflowing
from the hopper on the top of 02-D-326.
The separated oversizes fall by gravity into pulverisers (oversizes mill 02-Q-
301A/B/C/D), (one in each screening line) which consist on a double rotor mill with
chains, in a heavy duty construction and with rubber lined casing.
Those mills are existing. Only the by pass line have been reinstalled and the bottom
part of them have been modified to increase actual slope. In this way the settling
down of dust in this area will be reduced.
Undersize product from the four process screens falls by gravity, as well as
pulverized oversize product, to the recycle drag conveyor 02-M-304.
The recycle drag conveyor (02-M-304) will collect:

- The dust coming from all cyclone units.
- The crushed product from the pulverisers.
- Fines coming from process screens.
- Fines/oversizes from polishing screen
- Part of the commercial product which is in excess to required production.
New recycle belt conveyor (12-M-367) will collect:

- Recycle product from recycle drag conveyor
- Solids raw materials.
Final product treatment
On-size product leaving the product feeder belt conveyor (02-D-326) is fed to the
rotary cooler 02-M-363, which will cool down its temperature using chilled air. To
prevent absorption of moisture by final product during the cooling process, an air
desaturator 12-E-304 installed in series with air chiller 12-E-302 is also provided.
The necessary treated air flow for the cooling process is sucked from the cooler by
the cooler drum fan 12-C-306, which is equipped with an inlet damper to regulate
the amount of air. This fan is located down stream of cooler drum and cooler
cyclones.
In the air chiller 12-E-302, cooling agent is the ammonia which is working in a close
circuit. For this purpose a set of two compressors, ammonia separator and a cooling
tower have been installed to get air temperatures at the outlet of the chiller between
9-14C.
Some of NP/NPK grades have a critical relative humidity CRH of about 55-75% at
30C (lower at higher temperature) and they could retain moisture if ambient air
condition has a higher relative humidity. Air heater will increase air temperature and
consequently they will decrease air relative humidity, whereas air chiller will reduce
the absolute water content on incoming air.
Dust coming out with the air leaving the cooler is recovered in a battery of cyclones,
already mentioned, 02-D-324 and collected in their hopper, from where it is fed back
to the recycle drag conveyor 02-M-304.
After cycloning, gas will be sent to the inlet air to dryer drum (this duct has been
relocated).
Cooled product is fed by gravity to the product elevator 02-M-308, which has been
enlarged to allow feeding to the new polishing screen (12-F-302). In this screen,
double deck type, the remaining fines or the possible fines generated in the rotary
cooler and oversizes, are separated and sent back to the recycle drag conveyor 02-
M-304.
Commercial product leaving the polishing screen (12-F-302) is fed to Coater drum
(02-M-364),where the product in covered with coating agent.
This coating agent is coming from two places. In solid state (powder) from Coating
powder bin (12-D-327) fed by coating powder feeder screw conveyor directly in the
inlet chute from polishing screen (12-F-302) to coater drum (02-M-364). And finally
liquid coating agent is pumped from Coating oil tank, by new coating oil pump (12-P-
317), directly in coater drum bed.
This mixture of coating agents will protect, against the humidity, the storage of the
product; specially in those cases where urea is present and other NPK grades.
From Coater drum the product is sent to storage area by means of several belt
conveyors.
In Final Product Weigher (02-M-401) an automatic sampler is located to control the

quality of final product. This automatic sampler consists on a spoon than is rotating
at a very small speed and is taking during every hour several samples for a total
weight of not more than 5 kg.
In this belt conveyor, as well, a weigher (02-M-401) is installed to weight product

and to control the amount of coating agents to be feed in coater drum, by means of
controlling speed controllers in coating oil pump and coating powder screw
conveyor.
Gas scrubbing
A scrubbing system and several dedusting equipment are installed with the aim of
cleaning effluent gases as well as to recover nutrient elements from said streams.
The existing scrubbing system will be complemented with a new Granulator Pre-
Scrubber, 12-D-311A/B and a new Tail Gas Scrubber 12-D-312, to improve the
global efficiency and effluents recovery. This scrubbing equipment is a critical item
and will be designed by INCRO S.A.
With the installation of new equipment to complement the existing equipment, the
Gas Scrubbing System will be constituted by three washing steps :
First washing step will be composed by a single granulator/reactor Pre-scrubber 12-

D-311A/B, to which the gas stream coming from granulator and preneutralizer will
be fed.
It will consist of a low pressure drop duct scrubber, followed by a separation cyclonic
tower. Prior to the scrubber there is a rough washing of the gases in the duct
between granulator drum and this scrubber, with the main objective of keeping duct
always clean besides achieving a preliminary washing and saturation of the gases.
All the scrubber liquor used in the pre-scrubber and washing duct is collected by
gravity in the prescrubber bottom, which acts as a tank.
Re-circulation pumps 12-P-312A/B (one stand-by) would be sucking from pre-

scrubber bottom vessel.
Second washing step includes the three existing similar ventury scrubbers where
sprays in arms have been changed to improve washing efficiency and to avoid their
process & mechanical failure:
- Granulator Scrubber 02-D-301A/B, to wash gases coming from the new

Granulator/reactor Pre-scrubber 12-D-311A/B and sucked by the new exhaust
fan 12-C-301, installed downstream the scrubber. Ventury throat has been
enlarged to accommodate the larger handled flow with a reasonable pressure
drop.
- Dryer Scrubber 02-D-302 A/B, to wash gases coming from Dryer Cyclones,
sucked by the new dryer exhaust fan 12-C-302 installed downstream the
scrubber. Ventury throat has been enlarged to accommodate the larger handled
flow with a reasonable pressure drop.
- Dust Scrubber 02-D-310 A/B to wash gases coming from Dust cyclones, sucked
by the new Dust Fan 12-C-310 installed downstream the scrubber.
All these scrubbers are ventury type followed by a separation cyclonic tower.
Granulator and Dryer scrubbers share a common recirculation tank, equipped with
existing circulation pumps 02-P-302A/B and 02-P-305A/B for recirculation to ventury
scrubber and arm sections respectively.
An independent tank 02-TK310 with suction pumps 02-P-310/1 is installed for

dedusting scrubber 02-D-310 A/B.
Third washing step consists on a new tail gas scrubber 12-D-312, where the
streams leaving the mentioned Fumes, Dryer and Dust scrubbers will be washed
again.
The new Tail Gas scrubber includes a low pressure drop spraying area on its
horizontal feeding arm, followed by a double packing area. Four new pumps 02-P-
318 A/B/C/D (one stand-by) give service for the arm sprays and the two packing
sections.
With all these modifications the scrubbing system will fulfil the required emission
limits.
For the DAP and urea based NPKs production, given that our aim is the maximum
concentration of the slurries, it is advisable to limit the amount of water make-up to
the system, being preferable to work with more concentrated and lower N/P ratio.
For SAB NPKs production, using mixed PR&PN process, more water will be fed to
the reaction, and then N/P ratio in the scrubbing liquid can be higher, if required.
The normal liquid routing would be as follows:
A considerable part of the phosphoric acid is directly fed to the granulator/reactor

pre-scrubber 12-D-311A/B, where it is mixed with liquid coming from the second
step scrubber effluent tank 02-TK-302, mainly constituted by more diluted acid.
P2O5 fed to this first washing step (as phosphoric acid) and NH3 escaping from
granulator, pipe reactor and preneutralizer will react, so that the molar N/P into this
liquid will be about 0.3-0.6. Some quantities of sulphuric acid can be also added to
control N/P ratio and solubility. Reaction between sulphuric acid and ammonia is
stronger than the reaction with phosphoric acid and consequently it will take place
firstly.
Once most of the ammonia has been recovered in 12-D-311A/B, we can use a more
diluted acid for the second washing step, where the most important aim is to recover
evolved dust, apart from removing some of the remaining ammonia, with the
minimum fluorine emission. Make up of water to the scrubber effluent tank 02-TK-
302 is done from the liquid used in the final washing step (Tail Gas Scrubber),
mainly constituted of water with small amounts of nutrients.
In the Tail gas scrubber 12-D-312, the gases coming from second washing step, will
be washed, to carry out the reduction of the fluorine evolved during the phosacid
washing.
The raw water used in Tail Gas scrubber, after successive recirculations, would
contain a certain quantity of fluorine, which directly would create an equilibrium
concentration of fluorine in the exhaust gas over the required limit. A purge of water,
make-up of scrubber effluent tank 02-TK-302/310 will be made from tail gas
scrubber to avoid that problem
Provisions are made to feed small quantities of sulphuric acid to Tail Gas Scrubber,
via pH-meter, in order to achieve the most convenient pH (around 5) to enhance
both the fluorine and ammonia recoveries.
The liquid from the granulator prescrubber 12-D-311A/B, composed of the most
concentrated acid, will be split into the Pipe Reactor Feed Tank 12-TK-301 and the
Preneutralizer 02-R-303. In the P.R. feed tank it will be mixed with the rest of
concentrated phosphoric acid fed to the unit, not previously used in the scrubbing
section. To achieve the best mixing of the streams, this tank is equipped with an
agitator 12-M-315.
From PR tank three pumps 12-P-315A/B/C (one or two in operation and one or two
on stand-by) will feed the resulting phosphoric acid mixture to the Pipe Reactors 12-
R-301A/B.
In case of SAB NPKs production, most of the available sulphuric acid is directly feed
to the Preneutralizer.
Occasional overflows from tanks, or flushing of water for washings will be collected
in the existing sump tank, from where it will be returned to process by means of
sump pump.
The flow of liquids entering the unit will be automatically controlled and measured by
using the existing and new instruments. They will be included in a DCS control
system located in the existing control room.
Phosphoric acid and NH3 to pipe reactor will have an interlock device to shut down
and start-up before and after steam washing.
The new defoamer dosing pump 12-P-316 is provided to feed defoamer to the pre-
scrubber, main scrubber tank, preneutralizer and PR feed tank where phosphoric
acid is used, to prevent the formation of foams.
A new heating system will provide desaturated air to the different suction points of
the dedusting system, to reduce dust settlement on the dofified dedusting system
network.
2.2 MAIN CHARACTERISTICS OF T HE PLANT DESIGN AND OPERATION
2.2.1 Ammonia feeding
Ammonia will be introduced at battery limit in liquid state at -33C of temperature

and under pressure (always at least 3 kg/cm2 over the equilibrium pressure and 12
kg/cm2 as a minimum supply pressure), then preheated (in 12-E-301) to 0-5C and
finally distributed, still liquid, to the granulator ammonization ploughshares 02-M-
361, to the pipe reactors 12-R-301A/B, to the preneutralizer 02-R-303 and to the
ammonia separator 12-D-313 (for refilling purpose).
In the main ammonia line, as well as in the granulator ammonia line and in the pipe
reactor or preneutralizer ammonia lines, the pressure must be such as to keep the
ammonia liquid, that is, it will be higher than the equilibrium pressure at the
corresponding temperature. Table 2.2.1 shows some of the equilibrium pressure
values at different temperatures. PI-336 and TI-361, which are located on the main
ammonia line, will show respectively its inlet pressure and temperature.
The total amount of ammonia fed to the different equipments will be measured in the
following totalizers :
- Liquid ammonia to granulator ammonia sparger : FQ-335
- Liquid ammonia to pipe reactors A/B : FQ-333/334
- Liquid ammonia to preneutralizer : FQ-342
So, to know the total ammonia consumption, the three quantities, or only the used
flows must be added up.
Under ordinary operation the ammonia pressure at several points is as follows
- Inlet plant : 12 kg/cm2 (PI-336)

2
- Inlet granulator ploughshare 12-R-302 : 3-7 kg/cm (PG-330)
2
- Inlet Pipe Reactor 12-R-301A : 5-10 kg/cm (PG-329)
2
- Inlet Pipe Reactor 12-R-301B : 5-10 kg/cm (PG-328)
2
- Inlet Preneutralizer 02-R-303 : 2-8 kg/cm (PG-342)
2
- Ammonia separator (-) : 5-7 kg/cm (package supplier)
There is the possibility of a manual cleaning of the pipes at the granulator

ammonization ploughshares 12-R-302 and the pipe reactors 12-R-301A/B with MP
steam, and the possibility of a manual cleaning of the pipes to preneutralizer with LP
steam. There is also the possibility of cleaning the ammonization ploughshares and
its ammonia pipe with plant air. After cleaning 12-R-302 with steam, to avoid suction
of solids due to the condensation of the remaining steam inside the ammonia pipes,
the valve of air must be opened during 2-3 minutes to purge the mentioned steam.
All along the liquid ammonia feeding system there should be a safety valves in case
the liquid ammonia could be trapped. As it is known, ammonia vapour pressure
increases rapidly with the temperature (see Table 2.2.1), being it possible the
breaking of the line and the subsequent ammonia vaporization and leak to the
atmosphere. All those valves have been set to open at 18 kg/cm2 (g).
P&IDs P-06-12-300-005/006 show the valves and controls installed for the feeding
of ammonia to the different equipment. If these pipes were to be disconnected for
cleaning or maintenance, before the disconnection the pipes must be completely
drained of ammonia and swept with steam and water.
The ammonia flows will be controlled through the DCS system in the Control Room
by the FIC-335 for 12-R-302 (granulator ammonia sparger), FIC-333/334 for 12-R-
301A/B (pipe reactors) and FIC-342 for 02-R-303 (preneutralizer).
The measurements are made with mass type flowmeter.
Table 2.2.1
Ammonia equilibrium pressures at different temperatures.
TEMPERATURE C EQUILIBRIUM PRESSURE kg/cm2 (g)

-33 0
-21 1.41
-8 2.11
-6 2.40
-4 2.70
-2 3.06
0 3.37
2 3.61
4 4.03
6 4.45
8 4.85
10 5.30
14 6.18
20 7.74
30 10.89
40 14.85
2.2.2 Phosphoric and sulphuric acids feeding
The crude phosphoric acid is introduced in the granulation unit as a concentrated

rated of 48% P2O5 and measured with magnetic type flowmeters.
Once in the plant it is distributed to:
- The pipe reactor vessel 12-TK-301 through the FIC-337.
- The preneutralizer 02-R-303 through the FIC-341.
- The Granulator Pre-Scrubber 12-D-311A/B through the FIC-348.
- Scrubber seal tank 02-TK-302 (existing control)
- Dust Scrubber seal tank 02-TK-310 (existing control)
Phosphoric acid flows entering the plant during normal operation will be distributed
to the different points depending on the formula to be made. In Chapter 6 (DAP and
NPK manufacture), and also in Chapter 8 (Material balance) flows for each product
are shown.
The effluent liquid from granulator pre-scrubber 12-D-311A/B will be partially fed to
the P.R. Vessel 12-TK-301, where hot will be mixed with the remaining phosphoric
acid if required, and to the preneutralizer 02-R-303. This last only when producing
DAP or NP grades with high sulphuric acid content. Obviously, producing NPK
grades with PR process (PN remains stopped), all effluent liquid from pre-scrubber
vessel is sent to the pipe reactor vessel.
In general, the scrubbing system is fed with enough phosphoric acid and sulphuric
acid to retain the NH3 escaping the process. The mixture of this
phosphoric/sulphuric acid with the water fed to the scrubbing system through the
Tail-Gas Scrubber 12-D-312, will form the whole scrubbing liquid which will be used
to retain, not only the NH 3, but the dust and fluorine produced in the process as well.
It should be avoided to feed any excess of phosphoric and/or sulphuric acids to the
scrubbing system. Higher than required amounts of acid feed will originate a lower
scrubbing system N/P, that may help the escape of fluorine, and, also, being the
whole scrubbing liquid more concentrated in P2O5, it will evaporate less water in the
scrubbing process, limiting the total amount of water capable of being fed to the
system.
The opposite situation should also be avoided. A lack of phosphoric acid could lead
to increase the N/P value much more than the desired making it possible the
appearance of crystallization problems in the scrubbing system. Solubility tables

should be consulted to clearly understand the safe working areas.
In "Section 6.3 - Raw material and main utility consumption" are established, for the
different products, the amounts of water and concentrated and diluted phosphoric
acid to be fed, under ordinary operation, to the plant and their distribution.
Keeping the same amount of total P2O5 introduced as phosphoric acid according to
the formulation requirements, it would be possible to change the amount of water
fed to the system, bearing in mind not only the scrubbing system requirements, but,
more important, the adjustment of the liquid phase inside the granulator, in order to
obtain an optimum process: higher granulation yields, minimum recycle, minimum
fuel consumption in the drying process, better product quality, an easier operation,
etc.
The main lines handling phosphoric acid have some sampling valves that will be
used for the normal scheduled determination of its specific gravity, % P2O5, molar
ratio N/P, solids, % water, etc.
The periodic cleaning liquids of those lines will be conducted to the existing sump
tank present in the unit. To this tank will be also sent all waste and drainages
originated in the plant as a result of the cleaning of the acid lines and vessels,
occasional plant vessels overflows, etc.
The plant is also provided with 98% sulphuric acid feeding systems. All flows are
measured with magnetic type flowmeters.
Once in the plant it is distributed to:
- The preneutralizer 02-R-303 through the FIC-343.
- The granulator 02-M-361 through the FIC-336.
- The Granulator Pre-Scrubber 12-D-311A/B, through the FIC-347.
- The Scrubber Seal Tank 02-TK-302, through the FIC-351.
- The Tail Gas Scrubber 12-D-312, through the AIC(pH)-301.
2.2.3 Main Reaction
The equipment where the main phosphoric acid sulphuric acid and ammonia
reaction takes place is composed of a conventional Preneutralizer reactor, 02-R-03,
and the two installed Pipe Reactors, 12-R-301A/B. Main reaction is later completed
in the granulator solids bed, where more ammonia is added to get the final desired
N/P ratio, according the grade.
Preneutralizer si used to produce ammonium phosphate slurry in case of DAP

production and to produce ammonium sulphate/phosphate slurry when the plant has
to produce NP grades with high sulphuric acid content. In both cases, Pipe Reactor
is always used to produce the complementary slurry of ammonium phosphate,
according mixed process (PN+PR).
Pipe Reactors are used, one or both in parallel and keeping stopped the
preneutralizer, to produce all kind of NPK grades (not high sulphuric acid content).
2.2.3.1 Preneutralizer 02-R-303
This is a reactor of a conventional type.
The Preneutralizer reactor 02-R-303 will only be used in the manufacture of DAP or
15-15-15 or similar NP or NPK grades with high sulphuric acid content in its
composition.
Making DAP 18-46-0 with mixed PN & PR process, about 55-65% of the total
ammonium phosphate slurry will be prepared in the Preneutralizer under normal
conditions. Nevertheless all necessary slurry can also be prepared in the Pipe
reactors, if needed because of any preneutralizer shutdown or even in the PN if PRs
are not used, although in last case at lower production rate (75%)
Making 15-15-15, also with mixed PN & PR process, preneutralizer will made all
necessary slurry of ammonium sulphate and part of the slurry of ammonium
phosphate, meanwhile in the pipe reactor will be made the rest of ammonium
phosphate slurry. As the total amount of ammonium sulphate is so high, in this case
about 80-85% of the total slurries will be prepared in the preneutralizer, which
represents higher percentage than in case of DAP manufacture consequently in this
case slurry can be prepared in PN with only s slight capacity decrease.
The preneutralizer can be fed with phosphoric acid, sulphuric acid, acid liquor from
scrubbing system, water and ammonia, as it has been described before. Liquid
ammonia is fed to the bottom of preneutralizer through 3 nozzles located all along
of the circumference, to obtain the best distribution and reaction efficiency. The
preneutralizer is provided with an new agitator, 12-M-366, to improve the reactants
contact and the final slurry homogeneization .
In general, to improve ammonia reaction yield in the PN level should be around 60-
70%, but the higher it is, it increases the possibility of overflowing due to the foaming
that may be produced. There are two independent level indicators, LI-302 and LI-
303, with a series of alarms, to be carefully followed from the control room. Usually
this level will be between 55-65% of the total height of the preneutralizer. This level
can be adjusted changing the feeding to the reactor, although trying to keep the
proportions between the different feedings (phosacid, sulphuric acid, scrubbing
liquid and ammonia). The system should be stabilised keeping the balance between
inputs and outputs.
The slurry leaving the preneutralizer is transferred to the granulator 02-M-361 by the
existing slurry pumps 02-P-301A/B. There are two independent slurry tranfer lines,
each one connected to one of the pumps. The lines are steam traced in order to
keep the slurry temperature and, therefore, the required slurry fluidity. Each line is
provided with its respective set of magnetic flowmeters with a control valve and a
controller FIC-302/312, with recording in the DCS system as all feeding flows. In
case of a line blockage or maintenance of its pump, the other could be used while
the first one is washed with water and/or steam.
The preneutralizer temperatures are shown in the panel/DCS through a TI-369 that
has high and low alarm to detect any abnormality in the reaction.
This temperature will usually be between 110-120C making ammonium phosphate

slurry and between 120-125C making ammonium sulphate/phosphate slurry.
The vapours produced in 02-R-303 are sucked to the granulator pre-scrubber 12-D-
311A/B simultaneously with and independently to the gases sucked from the
granulator 02-M-301. In the suction line 950-EG-C45-102 (new line) from
preneutralizer, a damper is installed for the adjustment of the pressure required in
the reactor, achieving in this way the required aspiration.
The agitator support is independent from the preneutralizer body to avoid the
agitator being affected by the reactor vibrations due to the strong reaction.
It is important that the transfer lines steam tracing is operating all the time. There
are a series of steam traps which should be checked periodically. In case of
malfunction, they should be repaired as soon as possible.
If the plant is shut down for short periods of time, the preneutralizer can be kept full
of slurries, but LP steam would be introduced through the ammonia feeding nozzles,
checking before, manually, that the ammonia flows are closed. The steam will help
to keep the slurry temperature over 100C preventing too high viscosity and
possible damage in the agitator. If, despite the introduction of steam through the
ammonia nozzles, the temperature tends to decrease, there would be an additional
introduction of LP steam in the middle part of the preneutralizer body, through the
lines 50-S1-A1-a105/106-H.
Any time there is a serious risk of blockage in the preneutralizer due to the slurry
solidification, water must be immediately introduced, although controlling the total
flow fed. In this way, the slurry would be diluted and it would be avoided the
blockage of the whole slurry mass, which could mean a long plant stoppage and,
even, the need to use pneumatic hammers to unblock it.
It would be, therefore, convenient to systematically check, during operation, the

proper functioning of the preneutralizer, specially that there are not blockage
problems in the ammonia injection pipes, that the slurry temperature is stable, the
amperage consumption by the agitator is correct, etc. These ckeckings will avoid
any blockage risks in the preneutralizer.
2.2.3.2 Pipe Reactor 12-R-301A/B
Besides the Preneutralizer, the equipment where the main phosphoric acid and
ammonia reaction takes place, is composed of a two Pipe Reactors, 12-R-301A/B,
installed in the Granulator Drum 02-M-301 itself.
When mixed PN & PR process is used (DAP, 15-15-15...) the remaining slurry of
ammonium phosphate not produced in the Preneutralizer is produced in the Pipe
Reactor (about 35-45% in case of DAP and 20-25% in case of 15-15-15).
Depending on the grade, a considerable part of the whole reaction takes place into
the granulator solids bed, where the remaining slurries free acid and, eventually, the
sulphuric acid directly fed, are neutralized with ammonia.
The P2O5 of the formulation always comes from the phosphoric acid fed to the unit.
Totally or the corresponding part of this acid is partially neutralized with liquid
ammonia to a molar ratio N/P of 1.2-1.5, depending on the grade. Eventually, that
molar ratio range can be increased to 1.0-1.8.
The neutralization reaction mainly takes place in the Pipe Reactors, which are
installed so that the slurry of ammonium phosphate is poured directly onto the solids
bed of the granulator. This slurry has temperatures normally ranging from 130 to
155C and moistures content between 4% and 12%, depending on the grade and
the required granulation moisture in the granulator solids bed.
The Pipe Reactor is a tubular reactor developed by INCRO, S.A., of small

dimensions, that is composed of a mixture and reaction head to which the slurry
distributing tube is fitted. In the former, the phosphoric acid and the ammonia are
closely mixed, reacting and producing ammonium phosphate and the vaporization of
water. The reaction is completed along the distribution tube and the pressure in the
system propels the formed slurry, which is distributed directly over the solids bed
inside the granulator, at the same time that the steam and the unfixed ammonia
escape towards the granulator Pre-Scrubber 12-D-311A/B.
The ordinary operation range for each installed Pipe Reactor is between 10 and 25
t/h of ammonium phosphate slurry, and up to a maximum of 30-33 t/h in the DN80
PR and 37-40t/h in the DN100 PR.
The reactor's reacting head is designed so that a good mixture of the phosphoric
acid and ammonia is produced, achieving a high efficiency reaction.
Each slurry distribution tube has several slots (2 in DN80 & 3 in DN100) through
which the emerging slurry will be distributed. It also has, some collars or bracelets
that will totally or partially close the slots, depending on the operative capacity
required in the reactor and on the solids bed area on to which the slurry will be
poured out.
All those features give the system great adaptation flexibility, achieving a continuous
and stable reactor operation. Being, with this, the system pressure maintained
(usually around 2-4 kg/cm2), the reaction will remain practically constant without any
important local flash occurring that might produce an irregular discontinuous
functioning of the reactor.
The phosacid fed to PR is the partly ammonized phosphoric liquid coming from the
scrubbing system, although most times it is mixed with fresh phosphoric acid. The
flow to the reactor/s is controlled by the magnetic flowmeter FIC-338/339 which can
be regulated from the DCS system. Phosacid liquor is fed from Pipe Reactor Vessel
12-TK-301, by means of the Pipe Reactor pumps 12-P-315A/B/C. One or two of the
three pumps is used as spare, meanwhile one or two pumps in parallel will be
operated in case of production of NPK grades with Pipe Reactor process.
Each phosacid feeding line is connected to a steam purging that can be activated
with a switch HS-319/320, respectively for PR A and B from the Control Room,
so that it is possible to sweep the pipe reactor in case of an occasional blockage
being detected in it. Actioning the switch will give way to the steam at the time that
closes the phosacid acid, ammonia and purge pot drainage On/off valves and finally
opens recirculation On/off valves to pipe reactor vessel recirculation lines. After the
cleaning, the switch is turned off, closing the steam and automatically re-
establishing the ammonia and acid flows and the previous condition on close/open
the rest of On/off valves mentioned before.
Each switch HS-319/320 has three positions:
1 2 3
PR A PR B PR working PR flash PR Stop
Acid
FCV-338 FCV-339 O X X
HV-303 HV-304 X O O
Ammonia
FCV-333 FCV-334 O X X
Steam
HV-301 HV-302 X O O
HV-305 HV-306 O X X
O Open X close
The pipe reactor cleaning requirements are easily detected either by observing if the
acid and ammonia pressures tend to steadily increase (one or more flows are
reduced), or even by ear, as the slurry makes a characteristic noise when leaving
the reactor making it possible to detect any abnormalities in the slurry exit. This
cleaning procedure usually takes about 20-40 seconds, and, if the operation is
correctly performed, they are seldom required with this type of reactor.
To complete the acid neutralization to the final required N/P and N/S ratio,
depending on the grade and the sulphuric acid fed to granulator, an Ammonia
Sparger 12-R-302, is provided.
The sparger is ploughshare type with arms of minimum resistance to the bed,
through which liquid ammonia is fed very deeply into the bed and distributed
lengthwise and parallel to the granulator wall, so that losses of ammonia to the
scrubber are minimized.
Both items combined, P.R. and sparger, besides Preneutralizer, provide a great
flexibility on adjusting operation parameters in order to achieve a high efficiency.
In granulator, the use of ammonia in liquid state will also favour the control of
temperature into the bed, which is very important for products with urea and/or with
a high slurry/solid raw materials ratio in its composition.
No further reaction is necessary when using the INCRO, S.A process. Therefore, all
the reactions will be completed into the granulator and product leaving it will already
have the requested levels of N, P2O5 and K2O for the product.
Under ordinary operation the pipe reactor will operate within the following range
FORMULA DAP 15-15-15

Phosphoric Liquids
Feeding
%P2O5 43-46 38-47
Liquid Ammonia
Feeding
Slurry Molar ratio N/P 1.4-1.5 1.4-1.5
Temperature C
TI-366/367 130-150 130-140
Slurry Humidity
% H2O 7-14 4-10
This type of reactor, if needed, is, nevertheless, capable of operating with N/P
ranging from 1.0 to even 1.8, making ammonium phosphate slurry. The ammonia
losses will, however, increase as the molar ratio increases.
In these cases if a slurry humidity of around 5% is to be kept as the desired

maximum, together with temperatures under 150C, it will be necessary to adjust the
phosphoric acid dilution.
The pipe reactor is manufactured with materials that will withstand the corrosion that
might be caused by the products in its contact (SS 316-L, Uranus B-6, etc.).
2.2.4 Granulation
Reference is made to the P&IDs P-06-12-300-005.
The second important point where the reactions occur, after PN and/or PR reactors,
is the granulator drum.
The characteristics of this equipment and its process are as follows:
The ammonium phosphate or ammonium phosphate/sulphate acid slurries coming

from the pipe reactor 12-R-301A/B and from the preneutralizer 02-R-303 are
distributed inside the granulator drum over the solids bed, composed mainly, of the
recycled fine product and the solid raw materials fed. Those slurries are
ammoniated with the ammonia, fed through the ammonization ploughshares 12-R-
302 deeply into the solids bed.
The granulator drum is internally lined with rubber panels that, on rotating the drum,
can flex when they pass by the upper part, detaching any stuck product and leaving
the inside surface clean. This flexion is helped by the breathing holes of the drum
shell that permit the breathing, that is, the entrance and exit of air between the
panels and the drum shell.
As already indicated in 2.2.3, the steam purge for pipe reactor/s is done pressing the
corresponding hand-switch that will simultaneously stop the acid and ammonia
feeding flows.
As also already mentioned, the ammonia is fed to the granulator through an INCRO
designed ammonization ploughshares system. This is composed of four
ploughshares, each one carrying a DN 20 pipe through which liquid ammonia is
injected into the bottom of the solids bed through two lateral holes at their end.
These pipes are protected and supported by their respective ploughshares. The
ammonia is, thus, injected deep into the solids bed and with an exit parallel to the
drum wall, being, therefore, distributed all along the solids bed and achieving a high
ammonia retention efficiency. Each injection line has its own fast blocking valve in
case a particular area of the drum did not interest to be ammonized depending on
the process. The four ammonia pipes are fed through a common header to which a
steam and air line connects for the eventual cleaning of the injection pipes specially
at the beginning of the procedure or if a blockage is detected in them.
The ammonia is introduced liquid and cold, and, on reaching the ploughshares end,
some "flash" is produced which tends to chill the pipe even more. Thus, if the pipes
temperature tends to increase to room temperature this could be a sign of a
blockage in the exit holes. In this case a steam and/or air purge will be required for
1-2 min. In general, whenever there has been a steam purge some air should be
passed immediately after, or the steam remaining inside the injection pipes, on
becoming colder and condensing, may produce a suction effect of the solids from
the bed and block the injection pipes.
The slurry coming from the preneutralizer 02-R-303 is distributed over the solids bed
inside the drum through a single distribution pipe with several drills where spray
nozzles can be screwed. This pipe is connected to two independent pipes coming
from the two slurry transfer pumps 02-P-301A/B respectively. Through the
corresponding SC and FCV the slurry will be controlled from PN to granulator Each
line will have its own controls. Meanwhile, using its corresponding pump, the second
line/pump can be washed with water and/or steam.
It has also been foreseen the possibility of feeding part of the sulphuric acid needed
in the DAP and NPK production directly over the solids bed. This will be optional in
quantity, depending on the operation progress, and could help the granulation
process and to retain part of the ammonia losses the scrubber.
All pipes entering the granulator: the pipes from the pipe reactors, the pipe from
preneutralizer, the four ammonia pipes, sulphuric acid pipe and the water and are
supported by beam that crosses the drum from one end to the other and that also
serves as steam feeding pipe for TSP production.
Gases, vapours and dust coming from both the solids bed and the pipe reactor are
sucked towards the Granulator Pre-Scrubber 12-D-311A/B, by a suction duct
located on the product exit side, where they will be washed jointly with the gases
coming from the preneutralizer.
During the plant operation it is important that the operators observe the granulator's
performance in order to ensure that the solids bed and the granulated product are in
the proper liquid/solid phase and granulometry conditions. Section 6.6 explains the
plant operation and shows the right procedure to adjust those parameters and the
appropriate corrective steps to be taken, either by changing the recycle, the slurry
conditions, the slurry and ammonia distribution over the solids bed, etc. If this latter
is very wet and/or hot, it will tend to over granulate and vice versa.
On the product exit side the drum has a grizzly continuous with it. Thus, the product
leaving the drum, bouncing over the retaining ring will usually pass between the
grizzly bars towards the dryer 02-M-362 feeding. The product, however, some times
builds-up inside the granulator, or some product stuck to some granulator support is
detached, leaving the drum as a lump big enough as to be unable to pass the
retaining ring. For these cases a simple internal elevator was installed that, acting as
a lump kicker, lifts the lumps over the retaining ring and throws them to the rotating
grizzly. The lump will be now retained between the grizzly bars that, on rotating, will
tend to lift it and toss it, crushing it into small bits. This prevents any big lumps of
product from passing to the dryer and blocking the feeding chute to it.
The chute-box on the product exit side should have a series of inspection doors that,
during normal operation, will usually be kept closed, unless the granulation process
is to be observed. When these doors are closed, most of the air entering the
granulator and that is later sucked, will come from the product entrance side,
sweeping the granulator inside appropriately, and removing any vapours and dust.
On the product entrance side there should also be a door for the observation of the
drum (solids bed, slurry distribution, etc.), and a register door that allows the
entrance of air, in a bigger or lesser degree, which could enhance the solids bed
cooling, either directly or by producing an extra-vaporization of the solids bed water
with the subsequent additional cooling that this would produce.
At least two lights (one in each side of the granulator chute box) must be installed to
allow a good inspection and observation of the granulation process.
The product leaving the granulator will be periodically sampled for its temperature
control, pH and, if needed, analysis (see Section 4.1).
In case of blockage of the chute from the granulator to the dryer, the operator must
react very quickly preventing, with steel bars of the appropriate length, the beginning
of any build-up. It is of the utmost importance that close to the granulator there
should always be available two to four pneumatic hammers in good operating
condition, for the fast unblocking of the chute if this is completely blocked. If not, the
still hot and slightly humid product leaving the granulator, on cooling down, may
produce an enormous and very solid block that will require much more time to clean
and restart the process.
It should be tried to keep the mechanical components well lubricated at all times,
specially the attacking ring gear and pinion, otherwise, they will rapidly wear down
producing distortions and noises when the drum rotates.
2.2.5 Drying
The product leaving the granulator 02-M-361 has a free humidity of between 1.8%
and 3% that should be reduced to achieve the final product specifications (1.5%
maximum, but 1.2-1.4% more usually, depending on the grade).
The drying process takes place inside the rotating drying drum 02-M-362 into which
the product from the granulator enters by gravity through the feeding chute. Incros
design includes a full modification of the lifting plates along the dryer.
The drying temperature control, will be done as previous to revamping, and is made
by the automatic control of the natural gas entrance and of the relative amounts of
different airs that this implies, based on the gas temperatures at the exit of the
drying process or at the entrance of that process. For NP or NPK products without
urea, the entrance temperature could be higher and more variable depending on the
product humidity at the entrance, but will usually be between 100-150C (maximum
200C) and without exceeding 105C at the exit. In case of products with urea, if
some times are produced, that entrance temperature must be reduced to 100-120C
(maximum 140C), without exceeding 85-90C at the exit.
On the product exit side the drum has a continuous grizzly with a device that lifts
any product lump throwing it to a hopper that feeds the existing lump crusher (this
equipment should be repaired and put in on line). The crushed product is
incorporated to the product flow that leaves the dryer towards the screening area.
The gas flow at the dryer exit pass through the cyclone battery 02-D-322 sucked by
the dryer scrubber fan, located downstream of dryer scrubber 02-D-302A/B. The gas
flow is directed to the scrubbing system before being released to the atmosphere.
2.2.6 Screening and grinding.
The product leaving the dryer, a mixture of fines, oversizes and on-size product, is
directly fed to the screen product elevator 02-M-302 towards the screening section.
That elevator discharges to a diverter that equally feeds on to two drag feed
conveyors 02-DR-101/102 with two exits each one. So this allows to split the total
throughput of the dryer in four flows equivalent to 25% of the total; each one over
one existing screen.
The screening section is composed of four double deck type screens, 02-F-
301A/B/C/D.
The oversizes retained on the first screen deck (mesh will be changed by 4.2 x 15
mm) will fall by gravity into the Oversize Mills 02-Q-301 A/B/C/D, where they will be
crushed before being sent, by gravity, to the recycle drag conveyor 02-M-304.
The product pouring through the oversize screens mesh falls by gravity on the
second screen deck (mesh will be changed by 2 x 25 mm), where the fines are
separated and sent to the recycle drag conveyor (02-M-304). On size product is
sent, also by gravity, to the screen product conveyor 02-M-303 and from this to
Product feeder conveyor (02-D-326), where according the set point of the screen
product conveyor weigher (12-WQ-326) it is splitted in to final product to cooler drum
and recycle, by means of overflowing from product feeder hopper.
The required final product granulometric specification is 90% minimum between 1-4
mm and 80% or over between 2-4 mm. The operator should periodically check that
the screen cloths are not blocked, in which case they shall be manually cleaned.
Each line of complete screen system is designed to absorb up to 33% of the total
throughput, but it is generally more convenient for the best quality of the final
product to operate normally with the four lines working at the same capacity, splitting
nearly at 25% the flow coming from the exit dryer elevator.
The existing oversize mills are double rotor with chain type. Each mill has a
reinstalled by-pass tube to equilibrate the different pressures that the revolving
rotors create between the entrance and exit of mill.
Elevator, screens, feeders, etc, have revised dust suction points and ducts whose
collected flows pass through the dust vent cyclones 02-D-323, sucked by the dust
scrubber fan 12-C-310 after being scrubbed in the dust scrubber 02-D-310A/B.
2.2.7 Product extraction and cooling
Due to the high granulation yield obtained if the plant is correctly operated, the total
amount of on-size product obtained in the granulator will be higher than the required
plant production capacity. Part of this on-size product, mostly with a granulation
between 1-4 mm, will constitute the proper plant production.
The Product Feeder 02-D-326 will take the required amount of product from the
main granulation loop composed of the granulator, the dryer, screen transport
equipment, screening, grinding and return of the recycle to the granulator. There is a
weigher (12-WQ-326) that shows the weight of product over the Recycle Regulator
conveyor through a DCS system installed WICQ-314. It will be possible to change
the Recycle Regulator Conveyor speed depending on the WE-314 reading of the
weigher, through its variable speed motor.
The remaining not extracted on-size product will overflow and fall by gravity from the
Product conveyor Bin on the recycle drag conveyor 02-M-304, forming, together with
the fines the ground oversizes and the dust recovered in the cyclones, the total
recycled product.
Among all the different operation possibilities, the main objective is to achieve the
maximum granulation yield with the minimum recycle. This will give the maximum
plant production capacity.
Obtaining a good granulation yield with a minimum recycle will imply that the rest of
the system works correctly, bringing to the granulator bed the correct slurries (liquid
phase) and solids (solid phase), the required heat (produced by the in situ reactions
or delivered by the slurry) and obtaining the desired water vaporization from the
solids bed.
The on-size product coming from the granulation loop (after passing through the
recycle regulator), usually has a temperature between 85-90C. In order to keep the
final product in good physical state, it will be necessary to cool it down, otherwise its
surface will soften up enhancing its caking. This is especially true for the high urea
and/or KCl containing NPK products.
Also, if their temperature remains high during the storage, some reactions will
continue to take place in the granule surface, which could change their texture and
composition, enhancing the caking even more, the granules loosing their
consistency and, even, breaking down.
Thus, the installation will cool the product down to the maximum extent, using a new
chiller unit 12-E-302. The chiller unit have been designed as a closed circuit unit so
that means that we can cold down the product independently of the process used
(PR only or mixed process). In some cases to cool down the product is more critical
than others. In cases where urea or/and KCl are present if the product is not
properly cooled down during the storage period, it could partially desegregates into
the different compounds.
In this way, the on-size product coming from the recycle regulator weigher (12-WQ-
326) will pass through a Rotary Cooler (02-M-363), which is working with a flow of
air in counter-current with the solids stream, to reach the maximum efficiency.
The cooler is equipped with a cooler drum fan (12-C-306) that sucks the air required
for the cooling process. The air is passing through the chiller, desaturator unit,
cooler drum, cooler cyclones and finally through cooler drum fan. Then it is blown
directed to the scrubbing system before being released to the atmosphere.
NP and NPK products are hygroscopic, mainly if they have urea in its composition,
with a relative critic humidity (RCH) very low of about 55-70 % (at 30 C). Therefore
it should be avoided the product absorbing humidity from the air during the cooling.
For that reason an air desaturator 12-E-304 is provided. In this equipment the cold
saturated air leaving 12-E-302 chiller, is slightly heated (about 3-5 C should be
enough) in order to decrease its relative humidity to 50-70 % before being blown to
the cooler.
As a rule, all DAP/NP/NPK products should be cooled down to the maximum to

ensure that they remain in proper condition when stored for long periods of time.
The cooler has to be inspected some times in order to check that there are not any
product accumulations or build-ups in its flights. Is also very important to verify that
no air, or as minimum as possible, is entrying through the cooler inlet chute, in order
to assure that the maximum possible flow of cold air is coming from air
chiller/desaturator.
2.2.8 Polishing Screening and conditioning
The on-size and cold product leaving the rotary cooler 02-M-363, is transported by
the product elevator 02-M-308 to the last product treatment before it leaves the
plant.
The on-size product coming from the Rotary Cooler can still contain some oversizes
and fine product under 1 mm, not separated in the process screens or generated in
the rotary cooler itself, which will be separated in the polishing screen 12-F-302.
The polishing screen is of double deck type. This screen should be also provided
with cloth self-cleaning systems as in the case of process screens.
Good product from polishing screen, cold and free of fines and oversizes,
constitutes the final production and it is sent to coater, whereas fines and oversizes
are unloaded directly onto the recycle drag conveyor 02-M-364.
In coating drum the final product is conditioned before being storage. For that solid
powder and liquid coating agent are directly dosed over the product.
Powder is fed into the inlet chute from polishing screen to coater drum by means of
a screw conveyor (12-M-368), which is taking the powder from coating powder bin,
whereas liquid from coating agent tank (existing) is fed through 12-P-317 pump.
This liquid is spraying inside the coating drum by means of spray system (existing).
To control the amount of powder/liquid (whose ratio is more or less fixed with the
product) a final product weigher (02-M-401) is installed in final belt conveyor. This
weigher will control through RIC-306 and RIC307 the speed of screw conveyor and
coating oil pump to adjust both flows.
Finally to control the granulometry and quality of the product an automatic sampler
(12-SP-401) will be installed in final product conveyor. This will take small samples
of final product every programmed time in order to collect a complete sample to be
analyzed every 2 hours.
2.2.9 Main Fans
The granulation unit has three different groups of fans.
In the first group are the fans associated to the dryer combustion chamber. Their
controls and how to operate them is explained in the operation manual provided by
the supplier.
In the second group are the Cooler drum fan (12-C-306) and Dedusting Air Heater
Fan (12-C-305), to supply air to cooler and heated air to the dedusting system
suction points respectively. Their controls and how to operate them is explained in
their corresponding operating manual provided by the supplier.
Finally, in the third group are all the other fans in the plant and which are of higher
capacity, associated with the wet scrubbing system:
2.2.9.1 Granulator scrubber fan (12-C-301)
It sucks gases coming from the granulator 02-M-361 (including pipe reactor gases)
and from the preneutralizer (02-R-303). The aspirated gases pass through the
Granulator Fumes Pre-Scrubber 12-D-311A/B and Granulator Scrubber 02-D-
301A/B, being propelled to the tail-gas scrubber 12-D-312, before being released to
the atmosphere.
2.2.9.2 Dryer scrubber fan (12-D-302)
This fan is for the aspiration of dryer gases which, after passing through the
cyclones battery 02-D-322 and the dryer scrubber 02-D-302A/B are propelled to the
tail-gas scrubber 12-D-312, before being released to the atmosphere.
2.2.9.3 Dust scrubber fan (12-D-310)
This fan aspirates gases from the different points where dust is formed (dedusting
system): Gases, after being dedusted in the cyclones battery (02-D-323). flow to
Dust scrubber 02-D-310A/B, before being sucked by the fan, from they are propelled
to the tail-gas scrubber 12-D-312, before being released to the atmosphere.
All these fans have been designed with the required pressure and flow excesses to
allow a continuous plant operation for a minimum of two weeks before their eventual
turn off for a cleaning. During ordinary operation, dust will stick to and gather in the
ducts inner walls increasing the system's pressure drop. This increase is
compensated by a bigger opening of the dampers (up to 100% if needed) which,
initially, were partially closed. This measure will keep a constant flow allowing a
regular and satisfactory plant operation.
At the time of the cold start-up all dampers should be closed, being this shown in the
screen through DCS system. Each fan has an interlocking system that prevents the
start-up if the dampers are not closed.
The rationale behind the dampers complete closure is to minimize the instantaneous
power absorption during the start-up and to permit each fan to start working as
gradually as possible.
After the start-up and when the fans are steadily working and the system clean, the
dampers will be initially adjusted to approximately 60-80% open.
The degree of dirtiness in the system will be detected by the pressure drop between
the different installation points, and depending on which the manual additional
damper opening will be regulated.
The Granulator scrubber fan 12-C-301, the dryer scrubber fan 12-C-302 and the
Dust scrubber fan 12-C-310 are designed to be internally cleaned with water and/or
steam without having to open their casing. It is advisable, approximately once a day,
to let water and/or steam passes for about 5 min. This water or steam is sprayed to
the impulsor cleaning it from any stuck product. These fans have the corresponding
drainpipe for draining the cleaning waters to the sewer. Nevertheless it should be
verified that the drainpipes drain properly, otherwise water could be accumulated
inside the fans impairing their operation and even irreversibly damaging them.
2.2.10 Dust collection and recovery. Air preheating to dedusting system.
There are three different cyclone batteries: Dryer Cyclones (02-D-322) and Dust
vent cyclones (02-D-323) and cooler cyclones (02-D-324) for the recovery of most of
the dust (or very fine product) carried in the air or gas flows coming from the
different plant equipment.
The first battery, 02-D-322, will separate a great deal of the dust carried in the main
dryer flow. Then, gas flows to the scrubbing tower 02-D-302A/B (Dryer Scrubber)
where the remaining very fine product not retained and the small amounts of
ammonia that might come from the dryer are recovered by the corresponding
scrubbing liquids, which are then recycled to the process.
The second battery, 02-D-323, will separate the dust coming along with the
dedusting system air, that collects dust from various plant equipment, mainly
elevators, screens, crushers and conveyor belts. This air is aspirated by the Dust
scrubber fan 12-D-310, through the scrubbing system, where the very fine dust
product not retained in cyclones will be recovered.
Finally, there is a third battery, 02-D-324, that will separate small particles of dust
coming from the rotary cooler. This gas, suck from the cooler drum by the cooler fan
12-C-306, is sent back to the system through a injection in duct from combustion
chamber to dryer, forming together with the flow from combustion fans the total
drying flow.
With this, most of the dust generated in the process will be recovered, increasing the
plant yield and releasing to the atmosphere gas flows with a minimum of polluting
compounds.
The cyclones unload the retained dust onto collecting hoppers.
The hoppers and cyclone dust unloading is done through sealed air flap valves, the
product being unloaded onto the recycle drag conveyor 02-M-304.
All cyclones should be preferably insulated to avoid condensations and, in the case
of the 02-D-322 cyclones for the gases coming from the dryer, should be insulated
for personal protection reasons due to their high temperature.
All cyclones should be provided with up and down stream nozzles for sampling as
well as temperature and flow checks. Between the battery entrance and exit there
should be one PDI for checking the pressure drop through them. Under ordinary
operation, the estimated pressure drop of the clean cyclone will be of a maximum of
100-120 mm w.c. As the cyclones and entrance ducts are going to be loaded with
dust, the pressure drop will increase; when it reaches the 150-180 mm w.c. The
section should be stopped and the cyclones cleaned.
As the cyclones' pressure drop increases, it will be necessary to open the damper
of their respective fan to compensate for it and try to keep a constant air flow as
described in section 2.2.9.
The piping connecting both ends of the already mentioned PDI can be purged with
controlled amounts of dry air in order to keep it clean. Otherwise it will give wrong
readings.
Finally, if the hopper's unloading valves do not operate correctly and the amount of
dust unloaded is insufficient, the hopper and even the cyclone could be filled with
dust. If this happens, the pressure drop could easily drop below 90 mm w.c., in
which case the cyclone should be stopped, the system cleaned and the valves
checked.
The dedusting system has the possibility of injecting some preheated air propelled
by fan 12-C-305. This injection could be particularly useful on the high ambient
humidity days, to temper the transport duct walls and decrease the relative air
humidity inside, in order to avoid any possible water condensation on the walls and
to decrease the amount of dust that might be accumulated inside the system. Its use
is also advisable at the beginning of the operations to preheat the ducts before there
is any dust passing by them.
The injected air can be heated in the heater 12-E-305, using LP steam, being
possible to automatically control its temperature from TIC-354 included in the DCS
system. Air temperature between 75-100 C should be normally used to ensure the
above explained effect.
The air flow injected, however, should be controlled trying to avoid venting back in
any of the system points.
2.2.11 Scrubbing system
2.2.11.1 General
The production of granular compound fertilizer is accompanied by the release of

waste products that are potential environmental pollutants. These are mainly dusts,
fluorines and ammonia. The dusts are basically fed raw materials and fertilizer
product ultra fines. Fluorides, which evolve as the result of the process reactions,
are principally in gaseous state.
The ammonia gas and dust released during the production of DAP and all NPK
grades must be recovered for plant economy as well as for environmental reasons.
To recover these materials a scrubbing system is provided, which consists of
cyclones, venturi cyclonic wet scrubbers and final tail-gas scrubber.
Most of the dust generated in the processing of the fertilizer materials is captured in
high efficiency cyclone clusters and returned to the granulation process, via the
recycle drag conveyor 02-M-304. The fertilizer material dust not captured by the dry
cyclones is practically all removed from the carrying air in the wet scrubbing units.
2.2.11.2 Scrubbing system units
There are three scrubbing units.
The first step is composed of the Granulator Pre-scrubber 12-D-311A/B, for the
gases coming from the granulator 02-M-361 and from the preneutralizer 02-R-303,
mainly containing ammonia and dust.
It is a vertical section / cyclonic type scrubber. The washing liquid is normally

constituted by phosphoric acid (20-48% P2O5) and sulphuric acid. A considerable
part of the phosphoric acid is fed directly to the granulator pre-scrubber 12-D-
311A/B, where it mixes with liquid coming from the scrubber seal tank 02-TK-302,
mainly constituted by much more diluted phosphoric acid.
P2O5 and H2SO4 fed to this first washing step (as phosphoric and sulphuric acids)
and NH 3 escaping from preneutralizer, granulator and pipe reactor, react, producing
MAP and ammonium sulphate, so that the molar N/P into this liquid is about 0.4-0.6.
The addition of variable quantities of sulphuric acid can help to control N/P ratio and
solubility. Reaction between sulphuric acid and ammonia is stronger than with
phosphoric acid and consequently it takes place first.
The scrubber consists of two sections. The first section is a throat type venturi. The
pressure drops across the venturi are approximate to 200-300 mm of water column,
at which setting the near-micron and larger sized dust particles can be effectively
captured. The venturi bottom plates maintain a turbulent pool of scrubbing liquid for
erosion protection and gravity drain to the sumps ahead of the gas inlets of the
cyclonic scrubbers.
The second section is composed of a cyclonic section, which serve to disengage the
liquid droplets carried in from the ventury units.
Drain of vertical section is designed to eliminate the total amount of washing liquid
fed to that area. Also cyclonic part has a drain centrally located designed to
eliminate the total amount of washing liquids fed to scrubber. Both drains discharge
and join directly to the suction pumps 12-P-312A/B, from which the liquor is
recirculated to the scrubber, as well as being transfered to the preneutralizer 02-R-
303 and/or to the pipe reactor tank 12-TK-301.
From the Granulator Pre-Scrubber 12-D-311A/B, gases are then sucked to the
Granulator Scrubber 02-D-301A/B.
The second step is composed of the Granulator Scrubber 02-D-301A/B, the Dryer
Scrubber 02-D-302A/B and Dust Scrubber 02-D-310A/B; the first one for the gases
coming from the granulator pre-scrubber 12-D-311A/B; the second one for the
gases coming from the Dryer Cyclones 02-D-322, mainly containing dust and few
quantities of ammonia; the third one for the gases coming from the Cooler Cyclones
02-D-324 and dust vent cyclones 02-D-323, mainly containing dust and very few
quantities of ammonia.
All three scrubbers are similar scrubbing towers, venturi/cyclonic type, but, logically,
with different dimensions, according their respective gas flow. Those scrubbers are
existing ones and only new venturies throat and sprays nozzles will be installed
during revamping and modernization.
The washing liquid is always based in phosphoric acid solutions, but usually more
diluted than in the first scrubbing step (15-30% P2O5)
As most of the ammonia has been recovered in the first scrubbing step in the
Granulator Pre-scrubber 11-D-311A/B, we can use a more diluted acid for this
second washing step, where most important aim is to recover evolved dust, besides
removing some of the remaining ammonia, with the minimum fluorine emission. For
that reason, make up of water to the scrubber seal tank 02-TK-302 is done from the
liquid used in the final washing steps, mainly constituted of water with small
amounts of nutrients.
Drain of Venturi section should be large enough (new dimensions of 300 mm min for
all of them) to ensure total drainage of washing liquid fed to the Venturi. Also
cyclonic part has a drain centrally located designed to eliminate the total amount of
washing liquid fed to scrubber.
All liquids sprayed to the scrubbers 02-D-301/302A/B, drain by gravity to a common

reservoir, 02-TK-302, from which they are recirculated to the scrubbers by the
pumps 05-P-305A/B and 05-P-304A/B. Some part of this scrubbing liquor is
transferred to granulator scrubber 12-D-312A/B by 02-P-304A/B.
In case of Dust scrubber 02-D-310A/B the scrubbing liquor drains to Dust scrubber
seal tank 02-TK-310 and is recirculated by means of 02-P-311A/B. The same
pumps make the transfer to Scrubber seal tank 02-TK-302.
The third step is composed of the Tail Gas Scrubber 12-D-312, in which all gases
coming from previous scrubbing step will be washed again, to complete the gas
depuration process.
Tail gas scrubber 12-D-312 is composed by an horizontal duct scrubber, equipped

with several successive washing sections followed by an horizontal packed area.
The gases leaving the Dryer Scrubber 02-D-302A/B, together with the gases from
the Granulator Scrubber 02-D-301A/B and Dust Scrubber 02-D-310A/B, are
propelled to the Tail Gas Scrubber 12-D-302 by the Exhaust Fans 12-C-301, 12-C-
302 and 12-C-310 respectively, to carry out the reduction of their fluorine evolved
during the phosacid washing, as well as to complete the removal of remaining dust
and ammonia.
To achieve this goal the washing liquor is mainly constituted by water, slightly
acidulated with sulphuric acid to provide the more convenient pH for both ammonia
and fluorine recovery (arounds).
The pumps 12-P-313A/B/C/D are used to wash in the scrubbing unit and also for the
transfer of liquid to the dust scrubber seal tank 02-TK-310. The amount of process
water fed to the scrubber 12-D-312 is automatically regulated by means of the level
controller LIC-306, and it depends on the required water for preneutralizer and pipe
reactor reaction and the vaporized water in the scrubbing system.
The objective of this last scrubbing step is to comply with the strict requirements for
gaseous effluents. The water used in this step, after successive recirculations, will
contain a certain quantity of fluorine, which directly will create an equilibrium
concentration of fluorine in the exhaust gas over the required limit. To avoid that
problem, a minimum flow of liquid has to be drained from the unit and transferred to
the dust scrubber seal tank 02-TK-310. This drained flow is advisable to be higher
than 2.5-3 m 3/h.
The bottom area of the tail gas is used as three reception tanks in cascade for
pumps 12-P-313A/B/C/D suction. In the first reception tank provisions are made to
feed small quantities of sulphuric acid, via pH-meter ACV-301, in order to achieve
the most convenient pH to enhance both the fluorine and ammonia recoveries, as if
has been mentioned before.
Several PG (355/356/357/358) will be installed at the inlet of each spraying inlet line
to scrubber for controlling the flow to every packing step. On air side 5 PG will be
installed to control the pressure drop in each step. PG-350 before scrubbing in the
inlet arm. PG-351/352/353 after every packing respectively to control the rate of
dirtiness accumulated in the packing. When pressure is significantly increased from
one step to another those packing area should be dismounted and cleaned.
2.2.11.3 Scrubbing system control
The gaseous ammonia evolved in the various steps of producing DAP/NPK/NP must
be absorbed by the phosphoric and the sulphuric acids scrubbing media in the
primary and second stage scrubbers for all gases streams. Only minor quantities of
fluoride gases are evolved in the basic ammonization reaction section, but ammonia
recovery in the scrubber units is most effective at low pH values (that is, below 3)
and the reaction is exothermic, so that the scrubber solution temperature is
generally maintained between 55 and 95 C. At these conditions of pH and
temperature, fluoride gases are often stripped from the phosphoric acid before it
reaches the reaction system. Thus, the third stage, tail gas scrubber receives
fluoride enriched gases during the production. Because it is working at higher pH
and without phosphoric acid, the fluorine emissions will be in-significant in this third
stage.
The dust going to the scrubbers is about 0.6-0.9% of the plant throughput whereas, ,
the ammonia represents about 14-18% of the total ammonia feed, depending upon
the mode of operation. Therefore, to ensure good material efficiency, it is essential
that this equipment performs well and is carefully controlled.
All process water is added to the Tail Gas Scrubber 12-D-312 to keep the level
constant in its reception tank, which is controlled through the LIC-306.
The pH of the Tail Gas Scrubbing water is measured and adjusted by the pH-meter
ACV-301, connected to the sulphuric acid flow controller valve ACV-301, which
controls the sulphuric acid flow to the reception tank, to maintain a pH of about 4-5.
As told in the previous paragraph, the level of the tank is controlled by LIC-306
connected to Process Water valve (existing one). After being used as scrubbing
liquid, this washing water containing captured ammonia, dust and fluorine, is sent to
the dust scrubber seal tank 02-TK-310, being the flow controlled by LCV-302 valve,
connected to LIC-305, which is the level indicator controller of that referred Scrubber
Vessel level. A flow indicator, FI-344, installed in the transfer line, helps to operator
to know and evaluate the process water admission any time, from DCS system.
Liquid from TGS is transferred to the Scrubber Dust seal tank 02-TK-310, that
recirculates the scrubbing liquor from dust scrubber (02-D-310A/B), via LCV-302.
Phosphoric acid is added, through FIC-(existing). The vessel level will be controlled
by the LIC-305 (provided with high and low level alarms connected to DCS system
in the Control Room).
Part of the scrubbing liquor is sent to the scrubber seal tank 12-TK-302 by means of
the recirculation pumps 02-P-311A/B.
The scrubbing flow in 02TK-302 will consist on a mixture of washing liquor from
dust scrubber seal tank (02-TK-310), fresh phosphoric acid (from existing line and
control), sulphuric acid controlled by FCV-351 and recirculating flow from Granulator
scrubber (02-D-301A/B) and dryer scrubber (02-D-302A/B).
The flow recirculation to scrubbers is done by 02-P-305A/B and 02-P-304A/B, 305

pumps will spray in venturis and 304 in horizontal arms.
The level in scrubber seal tank in controlled by existing LIC and the transfer in done
by 02-P-304A/B from scrubber dust seal Tank.
The first step scrubbing liquor (the Granulator Pre-Scrubber 12-D-311A/B) is formed
by liquor from the second step scrubbing liquid, sulphuric acid added via FIC-347,
and phosphoric acid controlled through FIC-348. Sporadic defoamer additions will
be made through 12-P-316 A pump. Occasionally some clarified water could be
added through FI-307.
The 12-D-311A/B Granulator Pre-Scrubber level is measured and adjusted by LIC-

304 (provided with high and low level alarms connected to DCS system in the
Control Room) and controlled by the second step recirculating scrubbing liquor valve
LCV-301 to which is connected. In this way, level in 12-D-311A/B is always
controlled by the transfer flow coming from 02-TK-302. To know this transfer flow, a
flow indicator FE-346 is provided.
The control of the level is controlled in cascade mode trying to keep the level
constant, in any case this control can be done in automatic mode through this
system or the operator can set a transfer flow directly over the FIC-346.
Part of this first step scrubbing liquor is sent to the Pipe Reactor Tank 12-TK-301
and to the Preneutralizer 02-R-303, depending on the used process, by means of
the pumps 12-P-312A/B.
The following operating parameters should be monitored and controlled:
A. The gas-side pressure drop across the venturi scrubbers should be initially set
at the design value as shown on the pressure differential gauges. The pressure
drop adjustment is effected by manually adjusting the gas flow. During
operation this pressure should be controlled to detect any abnormality.
B. The total flow rate of scrubbing liquor to the scrubber sprays will be near design
values, since the spray nozzles themselves are orifices. The flows to the
scrubber sprays and venturis are intended to balance themselves.
The flow rates of liquor to the sprays are obtained when there is a minimum
pressure upstream of the nozzles of 1.0 kg/cm2. This upstream pressure can
range anywhere between 1.0 and 2.0 kg/cm2. The total flow rate of solution to
the scrubbing system is proportional to the circulating motor amperage, which
should be noted and correlated with the pump curve.
C. The cyclonic spray nozzles are subject to erosion and corrosion, as well as to
occasional plugging. Provision is made for the easy removal of these spray
nozzles for inspection and cleaning, or replacement, without shutting down the
scrubber system.
D. Inspection of the spray nozzles for the tail gas scrubber must be made
periodically. The total flow rate of the recirculating scrubbing liquid is a function
of the power input to the circulating pump at a given header back pressure;
thus, the pump motor amperage should be noted periodically and correlated
with the pump curve information. The pH of the circulating scrubber solution is
important for achieving low fluoride and ammonia gas emissions to the
atmosphere. Preliminary tests indicate that a pH around 5 must be maintained.
Provision is made for sulphuric acid addition, however, this should be checked
frequently to ensure meeting the strict emissions required without using
excessive reagent.
E. The manual external temperature checking of the scrubbing system piping will
reveal if there is any blocked pipe, as its temperature will drop.
F. The droplet separators, if installed, should be carefully inspected and eventually

cleaned. In case of blockage this would be detected by the system's pressure
drop increase.
G. The scrubbing vessel level should be kept at about 60-80% of a scale in which
the 100% will be the physical maximum possible. In this way there will be room
for eventual concentration corrections, N/P ratio, etc., by the addition of water or
acid (phosphoric or sulphuric).
2.2.12 Pipe reactor vessel feeding
The phosphoric liquid feeding to the pipe reactors 12-R-301A/B comes from the
Pipe Reactor Vessel 12-TK-301. This vessel, provided with an agitator, 12-M-365,
feeds the Pumps 12-P-315A/B/C (one remaining as stand by when two Pipe
Reactors are working). To this pipe reactor tank 12-TK-301 are fed the following
flows, which will constitute the phosphoric liquor to be fed to one or two pipe
reactors besides the corresponding ammonia.
- Phosphoric acid.
Part of this acid will be fed at this point for adjusting the P2O5 contents in the
final liquor. Its flow is controlled by FIC-337. The addition in this point is also
done to avoid too low N/P molar ratio in the scrubbing liquid, which can cause
excessive fluorine stripping into the granulator pre-scrubber.
- Phosphoric liquids from 12-P-312A/B (Scrubbing section)

Depending on the used process: PR or PN+PR. The totality or part of the
liquid advanced from 12-D-311A/B (the first washing step, composed of the
phosacid liquor, sulphuric acid fed to the first scrubbing step and the ammonia
and dust recovered in all scrubbing steps), is sent to the pipe reactor tank 12-
TK-301, where it mixes with the rest of fresh phosphoric acid fed to the tank,
not previously used in the scrubbing section. This flow is controlled by FIC-332
connected to PR Vessel level-meter LIC-301.
- Process water
Its use is eventual, only when a quick dilution of the acid in the vessel is
required by the process. When necessary, its flow is manually controlled.
Pipe reactor vessel 02-TK-301 is also provided with high and low level alarms
connected to the already mentioned LIC-301 and signalled in DCS system in
the Control Room.
The 12-P-315A/B/C Pipe reactor pumps have a line returning to the vessel in
order to avoid the stop/start when the PR stops, as well as occasionally to
help for the regulation of flow/pressure to the P.R.
- Defoamer
Defoamer is added to the PR Vessel, to prevent the formation of foams. It is
fed by means of the defoamer pump 12-P-316, the same pump used to feed
defoamer to the scrubbing system.
2.2.13 Liquids drainages
The plant should have a tank (sump tank) installed at 0.00 m level, to collect all
leakage collectors and plant scrubbing drains coming from the liquid handling area.
All of these effluents can be recovered and returned to the process.
2.2.14 Solid raw materials dosage
The solid raw materials that can be used in the DAP and NPK manufacture are
potassium chloride, ammonium sulphate, TSP, urea and filler. The type and
quantities are selected according to the manufactured grade and its specifications.
These raw materials are transported from stores to the DAP/NPK production area.
Five bins of large capacity to be used for Potash, Filler, TSP, Urea AS or spillages.
Raw materials bins 02-D-314/318A/318B/319 are equipped with five big blasters (air
knockers) working with plant air, to avoid product arching and accumulation inside
the bin.
A filter is also provided on the top of each bin, to avoid dust emission.
To control bins feeding from storage through DCS system in the Control Room, all of
them should be preferably mounted on loading cell type scales, which provide an
indication of the real amount of material contained inside the bin, through the weight
and the bulk density of each product.
Weight is converted into level measurement, with indication of low and high alarms.
Additionally a very high level switch should be installed, to provide a very high level
alarm, optionally interlocked with the raw materials feeding and connected to the
load area, to advise payloader operator to stop the feeding. This alarm will also
cover an eventual malfunction of the weighing cells or a misreading in case of a very
large product arching inside the bin.
It is important that the weighers are well calibrated in order to obtain and adjust the
required product grade. When the plant is working continuously, the weighers
should be calibrated at least once a week and whenever any decompensation is
detected.
At the bottom of each bin there is a manual bin gate to isolate the respective bin for
maintenance, if required.
Under each bin there is a feeder 12-G314/316/318A/318B/319, consisting on an

electronic weigher WICQ-307//311 and a belt conveyor, to automatically measure
and adjust fed quantities from DCS system in the Control Room.
Solid raw materials from feeders will be discharged by gravity on the new recycle
belt conveyor 12-M-367, which will discharge on the recycle elevator 02-M-305,
together with all the plant recycled solids.
All the conveyor belts in this section, as well as all the conveyor belts in the plant,
are provided with emergency switches as well as rotation and deviation controllers.
2.3 INTERLOCKING SYSTEM
2.3.1 Interlocking sequences
Table I at the end of this section shows all foreseen interlocks between the different
plant equipment. The interlocking system will now be briefly examined in order to
point out its peculiarities. Table I is fully comprehensive and should be carefully
studied to apprehend all its possible actions and details before starting the plant
operation.
In table I only the new interlock required for new equipment is shown in bold letter.
The normal letter is considered only for your information and should be in actual
Interlock system.
For the purpose of this study, the plant has been divided into different sections that
can work independently but whose equipment, within each one, is interconnected.
The final product section is composed of the Product feeder belt conveyor 02-D-326,
the Rotary Cooler 02-M-363 with its ancillary equipment, the Product elevator 02-M-
308, the Polishing Screen 12-F-302, Coating drum 02-M-364 with its ancilliary
equipment and the Final Product belt conveyor 02-M-401.
This later, discharges to store through successive final product belt conveyors,
located outside B.L., which we assume will be also connected to the interlock circuit.
The shut-down of any of that equipment will cause the shut-down of their
immediately previous feeding equipment.
The shut-down of the product feeder 02-D-326, going to the rotary cooler 02-M-363,
will not stop its product feeding from the process screens, since equipment belong
to the granulation loop. In such a case the on-size product will not be extracted and
therefore all incoming granules will overflow over the recycle drag conveyor 02-M-
304, through the product feeder bin overflow chute.
The granulation loop is composed of the Granulator 02-M-361, the Dryer 02-M-262,
the Screen Product elevator 02-M-302, the drag feed conveyors 02-DR-101/102, the
screen product conveyor 02-M-303, the recycle drag conveyor 02-M-304, the new
recycle belt conveyor 12-M-367, and granulator elevator 02-M-305. As in the
previous section, the shut-down of any of this equipment will cause the shut-down of
its immediately previous feeding equipment. Normally, crushers and screens will not
affect any equipment, in the same way that they are not affected by any. Therefore,
the recycle drag conveyor 02-M-304 shut-down will normally stop screen product
elevator (02-M-302) but not the screens nor their feeders. In this case, screens and
crushers will unload onto the shut-down recycle conveyor, which is not a problem,
as the feeding to that equipment has been suspended due to the shut-down of the
dryer that feeds them.
In most plants the granulation loop can be automatically started and shutdown in
such a way that the dryer will act as the surge reservoir. One recommended
automatic starting-up sequence of steps can be the following: granulator, granulator
elevator, new recycle belt conveyor, recycle drag conveyor, screen product
conveyor, drag feed conveyors, screen product elevator, and finally, the dryer.
Before, and independently, the mills, lump crusher and the screens will have been
manually started. Once the automatic starting-up is completed, the interlocking
system will be re-established.
Shut-down sequence will follow the reverse sense, starting from dryer and following
by the next equipment, till stopping granulator at the end.
Between the dryer and the granulator there should be an interlocking by-pass that
allows the granulator to be started while the dryer is stopped. Other equipment have
also by-passes in order to be able to be started independently from the rest. This
can be of help in certain situations, so that there is no need to start or stop the whole
unit.
Some granulation loop equipment are also interlocked with their ancillary equipment.
Thus, the dryer stoppage normally will automatically stop the natural gas entrance to
the combustion chamber, avoiding the product overheating inside it. The granulator
stoppage will stop, among others, the ammonia and slurries feeding as well as the
phosphoric and sulphuric acid flows to the scrubbing system and preneutralizer or
pipe reactor vessel. The existing by-pass will allow to continue with the addition of
the acids to the vessels in order to be able to adjust volumes or concentrations
during the time that the plant is stopped. At the same time it will open the steam
valves for the PR cleaning, preventing the slurries from blocking the PR head or
distribution pipe, and also it will be open the steam valves to the ammonia pipes to
preneutralizer to avoid its blockage because of slurry.
The new recycle belt conveyor shut-down will also stop all the raw material feeders
Finally, there is the gas scrubbing section with its scrubbers and their ancillary
equipment. We recommend that if the liquid recirculation pumps of dryer scrubber
stops, dryer combustion chamber should be also stopped, to prevent scrubbing
tower overheating risks. Although not recommended, in some factories local
regulations obly in case of scrubber pumps failure to shutdown fans, to avoid the
temporary leaking of gas to the atmosphere with slightly higher content of nutrients.
In case this interlock is installed, we will need a by-pass to enable to interchange
pumps A to B or B to A, without having to stop the plant. Nevertheless, since several
scrubbers are installed we do not consider this interlocking absolutely required.
Besides the main interlocks already explained, there are a series of other interlocks,
internal to the equipment or of the equipment with its ancillary elements, also
detailed in table I. For instance, the elevator motor will stop if the chain breaks or if
their rotation axis is blocked; the fans will not be started if the dampers are not
closed; the belt conveyors have also a rotation control and safety devices, etc.
Table I is provided to indicate which interlocks are required for the plant.
This tables should give a guide to wiring interlocks and should be followed. Any
changes to the interlock logic must be approved by INCRO.
The symbols used in the interlocking system are the following:

- SD: Shut down
- HT: High temperature
- FC: Fail close
- FO: Fail open
- CS: Close to start
- AS: Automatic start-up sequence
- ASD: Automatic shutdown sequence
- SS: Simultaneous start-up
- ISS: Impossible simultaneous start-up
- (B): By-pass with amber light
The Table I (interlocking system) is in the following pages.

BASIC ENGINEERING PT PETROKIMIA GRESIK DATE: Dec. 02
JOB N: 02-0012 INTERLOCKING SYSTEM
Equipment Item Action on unit by other Action by this unit on others
Granulator 02-M-361 S.D. by Dryer 02-M-362 (B) S.D. Recycle Elevator 02-M-305 (B)
S.S. with Lubrication Unit F.C. Ammonia Valves FCV-333/334/335/342 (B)
A.S.1 Automatic start up F.C. Sulphuric Ac.Valves FCV-336/343 (B)/ 347 (B) /351
A.S.D.9 Automatic shutdown (B)
I.S.S. with Dryer 02-M-362 ACV-301 (B)
F.C. Phosphoric Acid Valves FCV-337 (B) / 348 (B) / 341
(B)
Existing (B)
F.C. Slurry Valves FCV-338/339 / 332 (B) / 345 (B) /
LCV-301 (B) / 302 (B) / Existing(B)
F.O. Steam Valves HV-301/302
S.D. P.R. Pump 12-P-315 A/B/C (B)
S.D. PN Pump 02-P-301 A/B (B)
Recycle Elevator 02-M-305 S.D. by Granulator 02-M-361 (B) S.D. New Recycle Conveyor 12-M-367 (B)
S.D. by Zero speed SSL-
A.S.2 Automatic start up
A.S.D.8 Automatic shutdown
New Recycle Belt 12-M-367 S.D. by Recycle Elevator 02-M-305 (B) S.D. Recycle Drag Flight 02-M-304 (B)
Conveyor A.S.3 Automatic start up S.D. Micronutrients Feeder 12-WQ-314 (B)
A.S.D.7 Automatic shutdown S.D. Potash Feeder 12-WQ-316 (B)
S.D. by Zero speed SSL-306 S.D. TSP/AS Feeder 12-WQ-318 A (B)
S.D. by deviation switch ZS-306 S.D. Filler Feeder 12-WQ-318 B (B)
S.D. by Landyard sw itch HS-318 S.D. Urea Feeder 12-WQ-319 (B)
Micronutrients 12-WQ-314 S.D. by New Recycle Conveyor 12-M- None

Feeder 367(B)
S.D. by Zero Speed SSL-301
S.D. by Deviation switch ZS-301
S.D. by Lanyard switch HS -313
Potash Feeder 12-WQ-316 S.D. by New Recycle Conveyor 12-M- None

367(B)
S.D. by Landyard switch HS-316
TSP/AS Feeder 12-WQ-318 A S.D. by New Recycle Conveyor 12-M- None

367(B)
Filler Feeder 12-WQ-318 B S.D. by New Recycle Conveyor 12-M- None

367(B)
Urea Feeder 12-WQ-319 S.D. by New Recycle Conveyor 12-M- None

367(B)
Recycle Drag Flight 02-M-304 S.D. by New Recycle Conveyor 12-M- S.D. Screen Product Elevator 02-M-302 (B )
367(B)
S.D. by Zero Speed SSL-
S.D. by Lanyard switch HS-
A.S.4 Automatic start up
A.S.D 6 Automatic shutdown
Cooler drum fan 12-C-306 C.S. with its damper None

Dryer Fan 12-C-302 C.S. with its damper F.C. N.G. valve to Burner&Comb. Chamber 02-M-301
Granulator Scrubber 12-C-301 C.S. with its Damper Same action that the Granulator 02-M-361, except the
Fan shutdown of recycle elevator 02-M-305.
Dust Fan 12-C-310 C.S. with its Damper None
Dedusting Heater 12-C-305 C.S. with its Damper None

Fan
Product Elevator 02-M-308 S.D. by Coater Drum 02-M-364 (B) S.D. Coating Powder Feeder 12-M-368 (B)
S.D. by Polishing Screen 12-F-302 (B) S.D. Coating oil dosing pump 12-P-317 (B)
Coater Drum 02-M-364 S.D. by Final Product Conveyor 02-M-401 S.D. Product Elevator 02-M-308 (B)
S.D. Coating Powder Feeder 12-M-368 (B)
S.D. Coating oil dosing pump 12-P-317 (B)
Coating Powder 12-M-368 S.D. by Product Elevator 02-M-308 (B) None
Feeder S.D. by Coater Drum 02-M-364 (B)
Coating Oil Dosing 12-P -317 S.D. by Product Elevator 02-M-308 (B) None
Pump S.D. by Coater Drum 02-M-364 (B)
Pipe Reactor Pump 12-P -315 S.D by Granulator 02-M-361 (B) F.C. Phosphoric Acid Liquor Valve FCV-338/9
A/B/C S.D. by Granulator Scrubber Fan F.C. Ammonia Valve FCV-333/334
12-C-301(B) F.C. Phosphoric Acid Valve FCV-337 (B)
F.C. Scrubbing Liquor Valve FCV-332 (B)
F.O. Steam Valve HV-301/302
Polishing Screen 12-F-302 S.D. by Coater Drum 02-M-364 (B) S.D. Product Elevator 02-M-308 (B)
Combustion chamber 02-M-301 F.C. NG valve by Dryer Fan 12-C-302 Existing

Existing
Ammonia Valves FCV-335 F.C. by Granulator 02-M-361 None

F.C. by Granulator Scrubb. Fan 12-C-301
Ammonia Valve FCV-333 F.C. by Granulator 02-M-361 F.C. Phosphoric Acid Liquor ValveFCV-338
F.C. by Granulator Scrubb. Fan 12-C-301 F.O. Steam Valve HV-301
F.C. by Phosphoric Acid Liquor Valve
FCV-338
F.C. by Pipe Reactor Feed Vessel Pumps
12-P-315 A/B/C
F.C. if Steam Valve HV-301 opens
Ammonia Valve FCV-334 F.C. by Granulator 02-M-361 F.C. Phosphoric Acid Liquor ValveFCV-339
F.C. by Granulator Scrubb. Fan 12-C-301 F.O. Steam Valve HV-302
F.C. by Phosphoric Acid Liquor Valve
FCV-339
F.C. by Pipe Reactor Feed Vessel Pumps
12-P-315 A/B/C
F.C. if Steam Valve HV-302 opens
Ammonia Valve FCV-342 F.C. by Granulator Drum 02-M-361 (B)
F.C. by Granulator Scrubb. Fan 12-C-301
(B)
F.C. by PN Pumps 02-P-301 A/B (B)
Phosphoric Acid FCV-337 F.C. by Granulator 02-M-361 (B) None
Valve F.C. by Granulator Scrubb. Fan 12-C-301
(B)
F.C. by PR Pumps 12-P-315 A/B/C (B)
Valve F.C. by Granulator Scrubb. Fan 12-C-301
(B)
F.C. by PN pumps 02-P-301A/B

Valve FCV-existing F.C. by Granulator Exh. Fan 12-C-301 (B)
Phosphoric Acid FCV-338 F.C. by Granulator 02-M-361 F.C Ammonia Valve FCV-333
Liquor Valves F.C. by Granulator Scrubb. Fan 12-C-301 F.O. Steam valve HV-301
F.C. by PR Pumps 12P-315A/B/C
F.C. if HV-301opens
F.C by Ammonia Valve FCV-333
Phosphoric Acid FCV-339 F.C. by Granulator 02-M-361 F.C Ammonia Valve FCV-334
Liquor Valves F.C. by Granulator Scrubb. Fan 12-C-301 F.O. Steam valve HV-302
F.C. by PR Pumps 12P-315A/B/C
F.C. if HV-302 opens
F.C by Ammonia Valve FCV-334
Transfers Valves FCV-332 F.C. by Granulator 02-M-361 (B) None

FCV-345 F.C. by Granulator Scrubb. Fan 12-C-301
LCV-301/302 (B)
FCV-352
LCV-Existing
Steam Valve HV-301 F.O. by Granulator 02-M-361 F.C. Slurry valve FCV-338 if steam opens
F.O. by Granulator Scrubb. Fan 12-C-301 F.C. Ammonia valve FCV-333 if steam opens
F.O. by F.C. of Ammonia valve FCV-333, F.C. HV-305 with delay if steam opens
or F.C. of Slurry valve FCV-338 F.O. HV-303 if steam opens
F.O. HV-307 with delay if HV-301 if steam opens
F.C. HV-307 if steam closes
Steam Valve HV-302 F.O. by Granulator 02-M-361 F.C. Slurry valve FCV-339 if steam opens
F.O. by Granulator Scrubb. Fan 12-C-301 F.C. Ammonia valve FCV-334 if steam opens
F.O. by F.C. of Ammonia valve FCV-334, F.C. HV-306 with delay if steam opens
or F.C. of Slurry valve FCV-339 F.O. HV-304 if steam opens
F.O. HV-308 with delay if HV-302 if steam opens
Steam Valve HV-303 F.O. by HV-301 if HV -301 Opens
F.C. by HV-301 if HV-301 Close
Steam Valve HV-304 F.O. by HV-302 if HV -302 Opens
F.C. by HV-302 if HV-302 Close
Steam Valve HV-305 F.O. by HV-301 if HV -301 Close
F.C. by HV-301 if HV-301 Open
Steam Valve HV-306 F.O. by HV-302 if HV -302 Close
F.C. by HV-302 if HV-302 Open
PR recirculation HV-307 F.O. by HV-301 if HV -301 Open
line valve F.C. by HV-301 if HV-301 Close
PR recirculation HV-308 F.O. by HV-302 if HV -302 Open
line valve F.C. by HV-302 if HV-302 Close
Steam Valves PV-301 F.O. if Low Pressure in PAL-301 None
Sulphuric Acid FCV-336 F.C. by Granulator 02-M-361 (B) None
Valves FCV-343 (B) F.C. by Granulator Scrubb. Fan 12-C-301
FCV-347 (B) (B)
FCV-351 (B)
ACV -301 (B)

CHAPTER 3.- PREPARATION OF THE PLANT

INDEX
3.1 INITIAL PLANT PREPARATION AND CHECK
3.1.1 Mechanical equipment
3.1.2 Pumps
3.1.3 Agitators
3.1.4 Tanks , vessels and preneutralizer
3.1.5 Pipe reactors
3.1.6 Scrubbers
3.1.7 Ducts
3.1.8 Fans
3.1.9 Piping
3.1.10 Chutes
3.1.11 Electricity
3.1.12 Instrumentation
3.1.13 Flowmeters and weighers calibration
3.1.14 Safety valves
3.1.15 Miscellaneous
3.2 DAILY DATA LOG SHEET

3. PREPARATION OF THE PLANT

3.1 INITIAL PLANT PREPARATION AND CHECK
Once the plant is in working conditions, several checks should be performed in order
to avoid any future problems.
Although the time required to perform all the procedures we are about to describe
may seem a bit excessive, it is of the utmost importance that they are carried out
with the maximum rigour. Even if some of them seem repetitive, they will ensure that
everything has been checked. The time employed in this purpose will be largely
compensated by avoiding future shut-downs.
Other additional operations to be performed before start manufacturing, such as

loading and washing the PR vessels, filling the system with the initial recycle,
preparing the preneutralizer slurry (when it has to be used) and the start-up
procedure, will be dealt with in detail in section 6.5. These protocols will be the guide
for all subsequent manufactures.
It is advisable that in order to avoid any omissions, all revisions should be made
following a control list. This list should be prepared before hand and all items to be
checked should be orderly detailed. It also should have two specific places for the
person making the revision and his supervisor to sign on once the revision has been
completed. The final revision of all plant equipment before the start-up should be
made according to the following criteria.
3.1.1 Mechanical equipment
It should be checked that all mechanical equipment is well lubricated (gears, chains,
bearings, etc), as well as their amperage consumption, vibrations, noises, etc.
All couplings and screw-nut fastenings should be revised to check that they are
tightly fastened, as well as the strength of all weldings.
In case of any flanged joints, it should be checked that they are properly placed and
tight.
Every rotating equipment will be started individually to check that their rotating
direction is correct and that all motor connecting wires are properly connected.
In the Granulator, it should be checked that all its internals (ammonisation

ploughshares, acids, water and Preneutralizer /Pipe Reactor slurry pipes) are in the
right position and well fixed. It is particularly important to check that the distance
between the granulator ploughshares end and the equipment wall are the same as
the ones indicated in the corresponding drawings. It also should be checked that the
flexible rubber band surfaces are not damaged due to the assembling process. They
also should be checked for their flexibility.
The Pipe Reactors (PRs) will also be checked to see that they are properly placed
and fixed.
Screens will be checked at as many different vibrations as possible, as well as the

proper functioning of all belt/drag/elevator conveyors. All of them should have all
safety protectors and covers needed.
3.1.2 Pumps
It should be checked that they are well screwed to their bases, as well as the
incoming and outcoming piping lines, couplings, packings, sealings, etc.
Each pump should be individually started with water in order to check its rotation. At
the beginning, it will be checked that all temporary filters for the suction of the
washing system pumps and the acid feeding pumps to the PR are installed.
3.1.3 Agitators
It will be checked the lubrication, couplings and fastenings of each agitator. Also that
the motors are rotating in the right direction and that the amperage consumption is
within the limits expected for using water.
3.1.4 Tanks, vessels and preneutralizer
It should be checked that there are not any dirt or foreign bits of materials left inside
the tanks, vessels and the preneutralizer. Should there be anything left, it will be
removed before filling the tank.
All joints should be checked as well as the pipe connections and blind flanges
tightness.
It also should be checked that all submerged pipes are not clogged, and that the
instruments are properly placed.
Finally, it will be visually checked that there are not any flaws in their internal lining.
Should there be any, it will be repaired.
3.1.5 Pipe reactors
A first visual inspection of the slurry-distribution pipe should be made (with the
reactor head open) illuminating with a torch each opening spray of the distribution
pipe installed inside the granulator, and looking at it from the opposite side (the head
side). In this way we will be able to see whether there is any irregularity or residue
inside the pipe.
It should be checked that ammonia nozzles are ready to use and that they are
properly screwed to the F piece of the Pipe Reactor.
Finally, the reactor head will be assembled with the chosen ammonia nozzle and J
piece and the collars for all slots will be screwed to the distributing pipe, leaving the
corresponding opened area , for the immediate start-up.
It should be made certain that liquid ammonia and phosphoric liquor pipes to both
Pipe Reactors are properly installed.
3.1.6 Scrubbers
They should be inspected in the inside to check their condition, packing, paths,
lining, and that there are no assembly components left inside. The proper location of
the sprays should be checked as well.
3.1.7 Ducts
All plant ducts should be checked to ensure that they are well fixed to the supporting
structure. Seam joints and tightness should also be examined. All dampers should
be visually checked to ensure that they can operate at any opening, from completely
closed to completely open.
In due course, expansion gaskets will be installed between the ducts and ensure
that they are tight. It also will be checked that the pipe washing sprays are correctly
placed in the respective ducts.
3.1.8 Fans
They will be examined for their proper rotation direction. Amperage will be measured
by throttling the dampers at their inlet and checking that they work properly. They
will also be examined for vibrations, noises and the fastening to their base.
3.1.9 Piping
All plant flanged pipes should be checked for their tightness.
All pipe supports and their correct fastening shall also be checked.
Valves shall be manually operated to ensure that they can be operated in any
position, from completely open to completely closed.
3.1.10 Chutes
It will be checked that they are tightly fixed to the other plant structures or items.
Welded joints will be checked at their welding points, and screw joints will be
checked for their tightness.
In case of any lined chutes, it should be checked that the lining is in good condition.
3.1.11 Electricity
Before switching the main electric power on, the electrical department will have
made a complete check of readiness for all motors and electric equipment in the
plant.
3.1.12 Instrumentation
Loop checks shall be made by the instrument technicians, according to standard

practices, before attempting any operating activities.
All alarm circuits and devices will be turned on and checked, as well as all level
indicators and interlockings detailed in P&IDs and/or the Logical Interlocking
Diagram.
DCS software should be thoroughly checked to determine whether all

instrumentation interlock system operates properly.
3.1.13 Flowmeters and weighers calibrations
All meters should be checked before the plant start-up in order to ensure a good
control of all process parameters, raw materials and utilities consumption, yields,
etc.
For a correct checking, all meters calibration curves as well as correction factors
should be at your disposal (provided by the supplier) to be applied in case of
different product density, temperature, etc. As a rule, the instrument specialists will
follow the indications given by the suppliers for the calibration and adjustment.
The instrumentation department should record all calibrations done, keeping their
values for future checkings and/or modifications.
The plant liquid and solid material feedings will permit a verification of the calibration
in each of the meters.
A- Liquids
A-1 In case of error suspicion, phosphoric acid, washing liquids and sulphuric acid
meters will be checked through their corresponding meter at different flows,
either by collecting the liquids in a gauged vessel or by collecting the liquids in
a mobile tank lorry and checking the difference in weight before and after the
test in a calibrated weigher.
A-2 Due to the high temperature, viscosity and solubility nature of the ammonium
phosphate / sulphate slurries coming from the preneutralizer, their meters are
very difficult to check, and therefore they will only be checked if there is a
founded suspicion of a significant error in their measurement .
The procedure to follow for the checking of these meters is that of sending the
slurries to a container which previously will have been partially filled with water
to avoid the crystallization of the slurries when they get colder. The check will
then be made by the difference in weight, before and after the test , in a
calibrated weigher.
This procedure implies the connection of flexible hoses from the meter line to
the container.
A-3 Liquid ammonia. These checks will only be made in case of a well founded
suspicion of a significative error in the meters.
These meters can be checked sending the ammonia through a pressure hose
to a tank lorry and measuring the difference in weight in a calibrated weigher.
B- Solids
B-1 Raw materials weighers. They will be regularly checked with calibrated
weights, but from time to time they will be checked by sending the product to a
truck or container and weighing the materials in a second calibrated weigher.
B-2 The throughput weigher and the recycle regulator weigher will be checked by
using calibrated weights.
B-3 Final product weigher. It will initially be checked with calibrated weights. Its
final verification will be made later, once the plant is already started, loading
the product in a lorry and measuring the difference in weight.
3.1.14 Safety valves
Plant safety valves will be tested with limit, as from standard procedure.
3.1.15 Miscellaneous
Once all plant mechanical aspects have been verified, all pipes will be washed with
water. This should be done line by line, and not simultaneously. All necessary steps
should be taken in the off-sites to allow water to be sent to each piping line.
Each line will be filled with water at their inlet and then it will be pumped for 5
minutes with all valves completely open.
Once all the lines have been washed, their corresponding tank will be filled up to 30
cm below the overflow level. The valves will be closed and the agitators activated for
5 minutes to check for any liquid leak.
Then, the agitators will be stopped and the valve to the recirculation pump of the
corresponding washer will be opened. Each of the pumps in each washer should be
tested consecutively.
Once the pump suction line is full, slightly open the pump discharge and flow
regulating valves. Activate the pump and progressively open impulsion valves to
recirculate water through the washer for 5 minutes. In case there is not enough flow,
this may be due to remaining residues blocking the temporary filter. If this is the
case, close the inlet and outlet pump valves, disassemble the filter, clean it and
wash the line. Finally, install the filter again and start the recirculating process to the
corresponding washer.
Operate all recirculation pumps in a similar way for at least 5 minutes looking for
leaks. Once the procedure is finished, close all valves and remove all temporary
filters.
Once all washer pumps are tested, open each washer manhole and check whether
it has been damaged by any residues passing through the lines. In case of any
damage, it should be repaired.
If they have not already been washed, wash now the preneutralizer feeding lines,
including sulphuric acid line. Once washed, fill the preneutralizer with water, then
introduce air or water through the ammonia lines to the preneutralizer in order to
check all distribution tubes. Start the preneutralizer agitator for 5 min. to check its
good functioning. Now open the first slurry pumping circuit, including control valves,
and starting the pump , wash the line for 5 min. sending the water to a drainage
container and from there to a waste pipe.
Operate in the same way the second pumping circuit. In both cases, the slurry
access valves to the granulator will be kept closed. Once finished, open the
granulator accesses valves and washes the slurry lines and their collector distributor
inside the granulator for 20-30 sec. Then wash the lines and the slurry collector-
distributor from the preneutralizer to the granulator with LP steam.
The ammonia lines to the granulator, to Pipe Reactors and to the ammonia
separator will be washed in a similar way, as well as the water and acid lines to the
granulator. The same applies to the phosphoric acid, sulphuric acid and ammonia
lines to the Pipe Reactors and Preneutralizer. Finally their corresponding distribution
tubes will be washed with steam. After all these washings, pass air through the
ammonia and sulphuric acid lines for 5-10 minutes to dry these thoroughly.
At this time in the procedure, the preneutralizer should be completely emptied of

water and temporary filters protecting the pumps during the start up will be removed.
Inspect all equipment for solids, removing any residues.
All remaining circuits not mentioned (defoamer, etc.) will be washed with
compressed air or, alternatively, with water.
3.2 DAILY DATA LOG SHEET
To ensure a proper management of the plant, it will be needed to establish a control

system which is described in chapter 6, point 6.6. "Normal Plant Operation. Potential
Operative Problems".
The data obtained in these controls will be transcribed to the "Daily Data Log
Sheets" or "Daily Manufacture Bulletin" in order to be able to study all parameters
employed at a given time, and identify any deviations from the basic data.
CHAPTER 4.- GENERAL CONTROLS OF THE PLANT

INDEX
4.1 ANALYTICAL METHODS AND SAMPLING
4.1.1 Analysis to be performed in the plant

4.1.1.1 Liquids density
4.1.1.2 Slurries
4.1.1.3 Solids temperature
4.1.1.4 Solids pH
4.1.1.5 Liquids pH
4.1.2 Sample preparation and sampling
4.1.2.1 Solid raw materials
4.1.2.2 Finished product
4.1.2.3 Phosphoric and sulphuric acids and liquids in pipe reactor and scrubber
vessels
4.1.2.4 Gases
4.1.2.5 Dust emission in stack or ducts
4.1.3 Sampling and analysis frequency
4.1.4 Analytical procedures
4.1.5 Information for laboratory equipment
4.2 CHECKING AND CLEANING PROCEDURES
4.2.1 Revision and cleaning program

4.2.2 Main inspections in the equipment
4.2.2.1 Crushers
4.2.2.2 Pumps
4.2.2.3 Vessels and Preneutralizer
4.2.2.4 Pipe reactor
4.2.2.5 Granulator
4.2.2.6 Dryer and drying burner
4.2.2.7 Screens
4.2.2.8 Fans and cyclones
4.2.2.9 Scrubbing system
4.2.2.10 All other equipment and instruments
4. GENERAL CONTROLS OF THE PLANT
4.1 ANALYTICAL METHODS AND SAMPLING
4.1.1 Analysis to be performed in the plant
4.1.1.1 Liquids density
All acid densities, especially phosphoric acid, at their different streams will be
measured with a checked densimeter. At the same time the liquid temperature will
also be measured to correct the density value obtained and express it at 30 C, or
another pre-fixed temperature (usually 15 C or 20 C).
The density should be measured by taking with a measuring cylinder a quick sample
of 250-500 cc.
4.1.1.2 Slurries
A sample of the Preneutralizer slurry will be taken once every hour in order to
measure the density (at pumping temperature), pH and N/P molar ratio. The
Preneutralizer slurry density will always be measured at 95C, heating the sample to
this temperature if needed.
For the Pipe reactor slurry, being much more difficult to obtain a sample, it is usually
enough with the calculations of its N/P molar ratio from its feeding flows.
4.1.1.3 Solids Temperature
Solids temperature at the drums outlet and other eventual streams, will be
measured by getting a sample of 5-10 kg and transferring it to a box of the right size.
A checked ordinary thermometer will be introduced at different points until it reaches
the highest stabilized temperature.
4.1.1.4 Solids pH
Solids pH will be measured preferably with pH-meter, or at least with a sensitive pH

indicator paper (graded in 0.2 units) in a solution made with 10 g of sample
dissolved in 100cc distilled water. For this purpose a small container will be made
which, when filled to the rim, will contain approximately 10 g of granulated sample.
First 100 cc distilled water will be added to a gauged beaker and, then, the sample.
The suspension will be well stirred with a rod which will also be used to grind the
granulate.
After leaving it settle for 15-20 seconds the pH will be measured with the indicator
paper or the pH-meter.
Care should be taken not to make this measurement in an atmosphere containing

ammonia gas (for example, near granulator drum), which would distort the results.
4.1.1.5 Liquids pH
Liquid pH will be measured using the same equipment or indicator paper described
above.
4.1.2 Sample Preparation and Sampling
4.1.2.1 Solids raw materials
A series of boxes with a 4-5 kg sample capacity will be kept at each side of the raw
material hoppers. There will be a box for each different type of raw material in the
manufacturing process.
Every 2 hours, an instant partial 200 g sample will be taken manually. At the end of
the day there will be a 2-3 kg sample of each raw material.
Each sample will be mixed and then divided up to get several representative
samples of 200-300 g which will be used for the corresponding measurements.
Boxes should be kept closed between sampling to avoid cross-contamination

among samples.
4.1.2.2 Finished product
With the help of a continuous automatic sampler a representative sample of 3-5 kg

will be taken every 2 hours. This partial sample will be taken to the laboratory where
it will be homogenized and divided up until there are left two samples of 200-300 g
each. The first of the two samples will be used for the 2 hours control analysis (see
production control according to process). The second sample will be kept apart
along with all other successive 2 hours second samples until the completion of the
shift mean sample. This mean sample will be homogenized and divided up until we
get a 200-300 g sample which will be used for the chemical analysis. The rest of the
sample, discarded in the divisions, can be used for granulometry.
4.1.2.3 Phosphoric and sulphuric acids and liquids in pipe reactor and scrubber
vessels
Every 1 hour an instant 250 cc sample of each of the flows to be tested will be taken
and transferred to a container specifically prepared for this purpose. There will be a
different container for each flow and, if possible, plastic carafes should be used,
except for sulphuric acid, which must be inox type.
Every 8 hours, 8 samples of each flow will have been taken and they will constitute
the shift mean samples. Each carafe content will be homogenized by stirring and a
300-500 cc sample will be taken for the corresponding analysis.
4.1.2.4 Gases
A sampling device or analyser will be connected to the stack, in order to measure

any dust, fluorine and ammonia emission.
Sometimes another sampling points could be measured, to check the working

efficiency of the other former scrubbers.
The ammonia sampling device should have:

a) Glass wool filter.
b) Absorption bottles containing a solution of analytical reagent sulphuric acid.
c) Gas suction pump.
d) Flow-meter to measure the flow through the device.
After 4-8 hours, depending on the sulphuric acid quantity, the absorption bottles
contents will be recovered, homogenized and the retained ammonia measured.
Knowing the flow through the device, the gas flow through the ducts and the N
content in the washing liquid, it will be easy to determine the ammonia retention
efficiency.
4.1.2.5 Dust emissions in stacks or ducts
These determinations should be carried out by means of an isokinetic probe during

a short period of time (10-15 min.). In this way we will have instantaneous values,
but quite representatives, of the actual process performance.
4.1.3 Sampling and analysis frequency
Table 4.1 shows, as a guide, the recommended sampling and analysis frequency.
Obviously, the frequency can be changed according to the plant operation and the
raw materials higher or lower stability characteristics.
4.1.4 Analytical procedures
The analytical procedures for determining the raw materials and product quality,
including water content, nutrient content (N, P2O5, K2O) shall be as per "Official
methods of analysis for the Association of Official Analytical Chemists" (AOAC), or
equivalent as approved by OWNER. Product size testing shall be as per A.S.T.M. or
equivalent standards, as approved by OWNER.
4.1.5 Information for laboratory equipment
Apart from the common equipment for laboratory, such as flasks, pipets, etc., to
carry on the more usual determinations, the following equipment is recommended:
- Autoanalyzer (Technicon or equivalent)
The AutoAnalyzer is a continuous-flow analytical system. A continuously operating

peristaltic pump delivers samples or standard solutions and reagents to the
analytical system. A colour reaction then takes place in a heating bath or time delay
coil.
The stream is segmented by air bubbles, thus avoiding diffusion and preserving the
integrity of the individual samples. The residence of the samples -not only the
samples of unknown concentration but also the standard solutions of known
concentration- in each analytical unit of the AutoAnalyzer remains constant. It is
therefore not necessary for the end point of the reaction to be reached in each case,
since the degree of extinction of the unknown samples is always compared with that
of the standard. This mean that the AutoAnalyzer can produce extremely accurate
results in a short time.
The concentration is usually determined photometrically and is measured at steady

state. In this state the concentration of the analyse to be determined in the flowcell
remains constant. The peak height is proportional to the concentration of the
parameter to be measured.
It includes an specific circuit for each parameter to be analysed. Even for different
determinations of the same parameter, like total and soluble P2O5, an independent
circuit is used.
- Weighers of several precision grades

The laboratory should have weighers with a precision from the second decimal
up to the fourth decimal.
- Karl-Fischer apparatus
This equipment measures the water content of a sample, and has its basis in
the oxidation-reduction reaction which occurs between the water and the Karl-
Fischer reagent.
- Visible/UV Spectrophotometer
For the determination of anions in liquids the spectrophotometer in the
visible/UV field can be used. This technique is based on the absorption of
energy in the visible/UV range by a coloured compound. The intensity of light

transmitted through the sample is proportional to the concentration. Basically
there are two types of analyser, single beam or double beam, which is more
accurate. The last one provides excellent long term stability, reference
compensation and baseline correction.
- Flame photometer
Flame photometry is based on the measurement of the emission spectrum
produced when a solution of a metal is introduced into a flame. In the flame free
atoms are formed. The flame then excites the atoms and causes them to emit
radiant energy. This method is particularly useful for the determination of the
elements in the first two columns of the periodic table.
- Atomic Absorption Spectrometer

For components like boron, magnesium, copper, iron, ... , in case of production
of NP/NPK with trace-elements, we recommend the use of an atomic absorption
analyser. Thanks to the high accuracy of the latest models we presume there is
no need of a graphite furnace, unless concentrations in ppb are to be analysed.
Averagely speaking detection limit range from 15 - 150000 micrograms/litre,
depending on the selected element.
The analyser includes a photometer and a monochromator. A double beam,

time-shared and space-shared system is used. Light from the lamp is optically
chopped and passed alternatively through and around the sample
compartment; the beams are then recombined and travel through the
monochromator to a single photomultiplier detector. Its proven double beam
optical system provides the stability and reproducibility required for quality
automatic analysis. Front surfaced, reflecting optics with protective coatings are
used throughout for improved ultraviolet reflectivity and corrosion resistance.
Both the photometer and the monochromator are enclosed within protective
enclosures for further protection against corrosive environment.
- Inductively Coupled Plasma (ICP)

If the number of samples to be analysed is considerably high it is recommended
to use an atomic emission analyser. It can be used for simultaneous multi
elemental analysis. It detects the sample radiation emission instead of the
absorption, eliminating the need of several different lamps. This technique is
called Inductively Coupled Plasma (ICP) and consist on an argon Plasma
maintained by the interaction of a RF field and ionized argon gas. The sample is
introduced through the Plasma ring, confining it to a narrow region, thus
providing an optically thin emission source in a chemical inert atmosphere. This
results in a wide dynamic range and minimal chemical interactions in the
analysis.
- Kjeldahl apparatus
It is a distillation flask specially design for the determination of nitrogen.
- Stacksampler
It is a device for stack emission measurement. It is mainly composed of a probe
and a suction pump. The probe has a Pitot tube at the top of the probe for
isokinetic measurements and a filter for collecting the particles. The air passes
through several flasks with different reagents, where the pollutants are
collected.
- Sampling cup
This is a device for getting a representative sample of the product to be
analysed.
- Sieves
They are used to separate the product according to the different sizes of the
granules. It is recommended to have sieves of 1 mm, 2 mm and 4 mm at least.
- Hardmeter
This instrument measures the crushing strength for individual granules. The
compression tester can be manually worked or motor driven.
- Oven
This oven should reach the temperature of 120 ?C, and it is advisory to have
also an oven with a vacuum system.
- pH meters
- UV lamp
It is used for a qualitative checking of the anticaking recovering of granules, if
this treatment is done.
TABLE 4.1 (1)

SAMPLING PROGRAM
(See enclosed table for diagram keys)
Analysis Phosph. Acid TSP NH3 Sulph. Filler Potash AS

Frequency (48%) Acid
1 hour
2 hours 1 (c)
Once every 1 2 20 1 8
shift 2
9
20
Variable 3 (d)
4 (d) 8(a) 5 (c) 13 (d) 12 (a) 7 (a) 5 (a)
9 (d) 12(a) 8 (a) 8 (a)
13 (d) 4(a) 12 (d) 12(d)
14 (d)
15 (d)
16 (d)
17 (d)
18 (d)
19 (d)
(a) Every day, average sample

(b) Calculated from the PR entrance liquids
(c) Optional
(d) Every time a new raw material is used or every 15 days.
TABLE 4.1 (2)

SAMPLING PROGRAM
(see enclosed table for diagram keys)
Analysis Recirc.liq. Recirc.liq Recirc.liq. PN PR liq. PR

frequency 12-D-311A/B 02-D-302/310 12-D-312 Slurry 12-TK-301 12-R-301A/B
1 hour 1 1 1 1
10 10 10 20
11 11 11
20 20
2 hours 10 11
20 10
Once every 2 2 2 2 20 (b)

shift 6 6 6 6
8
Variable 9 (c) 9 (c) 9 (d) 2 (c)

7 (c) 7 (c) 2 (d) 7 (c) 6 (c)
6 (d) 9 (c) 8 (c)
7 (d) 10 (c)
18 (d) 11 (c)

(c) Optional
TABLE 4.1 (3)

SAMPLING PROGRAM
Analysis Granulator Dryer exit Final product Stack

frequency exit product product to stores gases
1 hour 12 20
20
2 hours 11 12 3
10 5 or 6
7
8
10
11
12
20
24
Once every 8 8 2 and 4

shift 11 5 or 6
7
Variable 20
21 (a) or (c)
22 (a) or (c)
23 (a) or (c)

(c) Optional
KEYS TO TABLE 4.1 PROGRAM
1. Specific gravity (at pumping temperature. For the Preneutralizer slurry, at 95C)
2. % P2O5, Total
3. % P2O5, Soluble in neutral citrate plus water
4. % P2O5, Water soluble
5. % N, Total (only in case of using Urea in the final product composition)
6. % N, Ammoniacal
7. % K2O, Total
8. % H2O
9. % Solids
10. pH
11. Molar ratio N/P
12. Granulometric analysis
13. % H2SO4
14. % CaO
15. % MgO
16. % Fe2O3
17. % Al2O3
18. % F
19. % SiO 2
20. Temperature
21. NH3 (ppm or mg/Nm3 )
22. Dust (ppm or mg/Nm3)
23. F (ppm or mg/Nm 3)
24. Hardness (kg)
4.2 CHECKING AND CLEANING PROCEDURES
4.2.1 Revision and cleaning program
A suitable revision and cleaning program of all the installation points has been
designed based on previous experience of the foreseen product manufactures, as
the equipment and product behaviour is not always the same.
It is advisable to keep a file of all the equipment, where all repairs and changes
produced will be recorded, as well as a break down and cleaning planning showing
all incidents affecting the different installation points. This will allow to have visible,
and easily apprehendable, all incidents and the stoppage length they caused, which
is very important in order to analyse the repetitive incidents and study the possible
corrective measures.
Nevertheless, and as reference, enclosed Table 4.2 shows an approximate program

to use from the start-up.
4.2.2 Main inspections in the equipment
During the plant operation all chutes, piping, etc., will be regularly inspected. These
inspections include the maintenance revisions and should be systematically
performed, according to a thoroughly defined revision program of the type indicated
in the previous paragraph. This program will have been designed by the Plant
Maintenance Department in base to this Operation Manual and bearing in mind the
special operation instructions given by the equipment suppliers.
Thanks to these inspections any needed repair will be detected, some of which, if
important, may require the plant emergency shut-down. If this was not the case, the
repairs will be programmed for the next scheduled plant shut-down.
Next, and without being very extensive, are indicated the main problems and the
corresponding revisions to be performed in some of the plant main equipment to
which this Manual refers to.
4.2.2.1 Crushers
Crushers are subject to vibrations, adherence and product build-up inside them and
in their mobile parts, chains or other crushing elements wear-down, bearing
problems, etc. The vibrations and amperage consumption can give an idea of their
operation condition.
It is recommended to inspect them once per shift. They are recommended to be

thoroughly cleaned once a week. The vibrational problems are usually caused by
the dynamic unbalance of the mobile parts, due, occasionally, to structural faults,
and, frequently, to product build-up and adherence. This build-up, although usually
quite uniform, can be partially detached by any sudden change or movement,
producing unbalances that will cause vibrations. For instance, this usually happens
when starting a crusher that has been temporarily stopped. That is why it is best to
always keep the crushers in operation, unless the plant is going to be shut-down for
a long time.
When the vibration cannot be obviated, the crusher should be stopped and cleaned.
In any case, the crushers will be thoroughly cleaned during the scheduled plant
shut-downs.
4.2.2.2 Pumps
The Preneutralizer slurry transfer pump is one of the key points in the DAP or NPK
manufacture when mixed PN+PR process is used (or, obviously, using only PN
process). This slurry is corrosive and erosive due to its acid nature and solids
content.
During normal operation, the pump will be changed at least once a day (better still
once a shift) for the stand-by pump, cleaning the former and its corresponding line
with water and steam until they are clean.
The recirculation and scrubbing liquids transfer pumps, although subject to a lesser
erosion due to their smaller solids content, will also be corroded by the acid liquids,
more or less hot, that they handle.
Also, the lines are subject to blockages and product adherence, specially if part of
the operation has taken place under abnormal conditions, i.e., with an excessive
N/P molar ratio, excessive solids content due to a cyclone malfunction.
Thus, it will be also convenient to change periodically operating pump for the spare
one, in order to clean it. During the weekly plant shut-down, the recirculation and
transfer lines as well as the tanks will be thoroughly cleaned, being well inspected
and repairing them if needed.
Mechanical seals cooling water should be checked.
4.2.2.3 Vessels and Preneutralizer
During the scheduled plant shut-downs, the vessels will be cleaned with water, and
the agitators and baffles inside them checked.
When the Preneutralizer is emptyed, usually once a month or every time that mixed
process is changed to a PR process (PN has to remain stopped) or even during a
long plant stoppage, it will be thoroughly cleaned and the agitators baffles and
reactors body examined, specially in the area near the sulphuric acid feeding,
checking that it is not corroded. During the PN operation, it will be checked that the
liquid ammonia nozzles are clean. If the ammonia nozzles feed line pressure tends
to go up, it will mean that the nozzle are not clean, and steam should be injected to
clean than If the liquid ammonia nozzle feed line tends to heat up, it will mean
nozzle blockage and also steam should be injected for cleaning.
All agitators amperimeter, mainly the Preneutralizer agitator will be regularly

observed during operation, and its readings will be recorded at least once per shift.
These readings will be indicative of any change in viscosity, concentration, solids
percentage, etc., in the slurry or scrubbing liquid, or of any mechanical anomaly. In
this last case , specially if the anomaly is detected in the PN agitator, sometimes it
might be necessary an emergency plant stoppage, to avoid serious mechanical
problems.
It is advisable to steam-sweep the PR once per shift, to ensure that the slurry exit
slots in the distribution pipe are open.
Periodically, the reactor's head will be disassembled, and examined that the
distribution pipe inside is clean.
Cleaning frequency will depend on the quality of phosphoric acid used. If it contains
many impurities, cleaning frequency will increase.
To prepare a good, efficient and quick cleaning, it is advisable to set a screw type
mechanical device, like the ones used to clean boiler pipes.
4.2.2.5 Granulator
It will be checked that the slurry distribution pipe from the Preneutralizer and also
the installed sprays functions properly, passing steam in case of blockage.
On the plant shut-down days the granulator's interior will be cleaned, and the
distributing pipes of slurry and sulphuric acid checked and carefully cleaned,
disassembling it if needed.
The chutes, either at the product inlet or outlet, should always be clean. During each
shift, there will be a more thorough clean without stopping the installation, by using
rods and/or pressurized water.
By the temperature of the ammonia ploughshares feeding pipes it will be possible to

detect if there is any blocked pipe, in which case it will be cleaned by passing steam
for 1-2 min. It should not be passed for longer periods of time in order to not to past
the granulator's bed with the steam condensate entering the granulator. If the steam
was not enough, the pipe will be opened during the next stoppage. If there was a
problem with more than one injector, or only with one but necessary for the
operation, the plant will be stopped and the injector unblocked. After passing steam
do not forget to immediately inject plant air or ammonia, to avoid vacuum inside the
ploughshares and ammonia pipes due to residual steam condensation. If this
happens, solid product from granulator bed can be sucked and the ammonia pipe
blocked.
During the operation the drum amperage consumption will be observed. It will be
indicative of the instantaneous load in it, and, in some way, of the state of the
production inside: if the production tends to build-up or to stick to the ploughshares,
increasing the internal friction, the consumption could be increased. Also, it could be
indicative of any mechanical anomaly or lack of proper lubrication in the ring gear,
tires, trunnions, rollers, etc.
In case of any product build-up inside the granulator that might impair the operation,
the drum will be stopped to be better observed, and if it is nothing serious it will be
started again. Frequently, the simple fact of stopping and starting the drum may
cause the build-up disgregation. If this was not the case, and the operation became
more difficult, the installation will be stopped and the build-up manually disgregated.
Once a week, all the product stuck in the drum internals will be thoroughly cleaned,
and the condition of the flexible rubber panels and their flexibility examined. Also, it
will be checked the grizzly bars at the product exit.
4.2.2.6 Dryer and drying burners
As in the granulator, the electric consumption will be checked. This reading will also
be indicative of the dryer load, which will inform of any product retention due to a
change in its granulometry and moisture. Working in high wetness conditions could
produce a temporal amperage increase, as well as a permanent one, in spite of re-
establishing normal operation conditions, due to the product sticking to the dryer
flights. In reference to this, it will be tried that the dryer entrance chute is always
clean. Each week it will be thoroughly cleaned, as well as the product pushing spiral
flights located in the drum first part. Any obstruction or blockage in these can cause
an overflow outside the drum of the materials that are not being pushed in, or a
estrangement of the canal going down to the granulator, which will require suddenly
stopping the granulator with the subsequent problem of hardening of its contents
due to the lack of the drum rotation.
As a rule, the combustion chamber refractory does not tolerate fast overheating or
cooling down without cracking. When the burner is to be stopped, and whenever
possible, the temperature will be first dropped, decreasing the natural gas feed for
about 10 min. The lighting should also be done gradually. Sometimes, however, due
to an emergency situation, the stoppage (and chamber cooling) will be done quickly,
having then to carefully examine if there has been any damage.
The refractory can still work with small cracks, but the big cracks have to be
repaired, or the chamber body may be seriously damaged. All instruments and
interlocks will be examined weekly.
4.2.2.7 Screens
If despite the automatic cleaning mechanism any cloth becomes blocked, it should
be cleaned by the operator as soon as possible. Besides that, and at least once per
shift, they will be inspected and/or cleaned.
If any abnormal hole was observed in the cloth, it should be repaired during the next
plant stoppage.
From time to time, the cloth tension will be checked as well as the system's
vibrations.
4.2.2.8 Fans and cyclones
As the system operates its pressure drop will increase due to the product deposits
inside the ducts, fans, cyclones, etc... This will be compensated by increasing the
corresponding damper opening.
The Granulator Scrubber fan, the Dryer scrubber and the Dust scrubber Fans will be
periodically cleaned without having to stop the installation. This will be done
spraying water and/or LP steam for 5-10 min. Longer sprayings should be avoided
in order to not to damage the fans. The other fans will be normally cleaned when the
unit shutdowns or when needed.
The fans electric consumptions will also be checked, as they will be indicative of
how the system is going.
In the cyclones, the flap valves located at the bottom of the hoppers, will be carefully
checked for their proper unloading and good sealing, otherwise too much dust will
pass to the scrubbing section causing the scrubbers' blockage and having to stop
the plant.
During the plant shut-down days, the cyclones and hoppers will be opened and
inspected, cleaning them if needed.
4.2.2.9 Scrubbing system
Every two hours approximately, the liquid flows to the scrubbers will be checked. In
case of any blocked spray, it will be detected because its feeding pipe will be cold,
or because the flow will decrease and the pressure increase. In these cases, they
will be cleaned. To avoid this happening, the flows should never drop in more than
15% of their normal values.
In the opposite situation, if there is a pressure drop in the spray feeding line, and the
pump is working properly, but its flow is equal or higher, it could be that a spray has
been lost. This will be checked and, if needed, repaired.
If the scrubber normal pressure drop increases in 50 mm w.c., this will be indicative
of a product build-up in their interior. If the increase was over 100 mm w.c., they will
be cleaned.
On the plant shut-down days, the scrubbing drain pipes to their tanks should be
cleaned.
Each week, approximately, or on the shut-down days, the recirculation pipes and
scrubbing system sprays will be cleaned with water.
4.2.2.10 All other equipment
For the rest of the equipment, the standard care and maintenance instructions will
be followed, as well as those recommended by the suppliers.
In general, all instruments should be calibrated at least once a month, and the
weighers once a week.
On this point, it is advisable to record all calibration data to have them available to
be checked at any time, being it possible to establish a plan to follow, and its
frequency, depending on the recorded data.
TABLE 4.2 (1)

REVISIONS AND CLEANING PROGRAM
ITEM FREQUENCY
8h 1 day 1 week 1 month 6 months
Solid raw materials bins 1 4
Solid raw materials weighers 1 4, 8 9
Final product weigher 1 4, 8 9
Granulator (*) 1, 10 11, 4, 5
Inlet Chute to Granulator (*) 3, 1 4
NH3 Injectors to Granulator 1 4 7
Acid distributing tubes into Granulator 1 4 7

Granulator Grizzly 1 4
Granulator internal lining 1 4 7
Reaction head (PR) 1, 3 4 9
Distribution tubes (PR and PN) 1, 3 4, 9
Preneutralizer PN 1 4
NH3 Injectors to PN 1 3 4
PN agitator 10 1, 5 4
PN slurry pump (plus piping) 10 1, 5, 12 9 7
Dryer (*) 10 1 11 4
Dryer inlet Chute (*) 1, 3 4
Burner (*) 1 9 11 4, 8
Grizzly (*) 1 4
Screens (*) 1,3,10,13 5 4 7
Crushers (*) 1, 10 5 4 7, 9
Recycle product weigher 1 4, 8 9
(*) In case of present maintenance program is more restrictive than this one keep the existing one.
KEYS TO TABLES 4.2 (1,2)
1- Operator routinely visual inspection

2- Cleaning inspection while the equipment is on operation
3- Equipment cleaning while in operation
4- Installation thorough cleaning
5- Abnormal vibrations checking
6- Elongations regulation and verification
7- Used internals replacement (boosters, chains, screen cloths, flexible panels, etc.).
8- Calibration and ruling
9- Internals inspection
10- Motor consumption checking
11- Visual inspection of the inside and removal of the deposits.
12- Change for stand-by and cleaning of the stopped equipment.
13- Verification of the vibrators correct functioning.
CHAPTER 5.- PLANT SAFETY

INDEX
5.1 INTRODUCTION
5.2 AMMONIA
5.2.1 Generalities
5.2.2 Safety regulations
5.2.3 Safety equipment
5.2.3.1 Ordinary use equipment
5.2.3.2 Emergency equipment
5.2.4 First aid
5.2.4.1 Ammonia inhalation
5.2.4.2 Ammonia ingestion
5.2.4.3 Skin contact
5.2.4.4 Eye contact
5.2.5 Working in ammonia containing atmospheres
5.2.6 Leaks
5.2.6.1 Detection
5.2.6.2 Repairing
5.3 PHOSPHORIC AND SULPHURIC ACIDS

5.3.1 Generalities
5.3.3 Safety equipment
5.3.4 First aid
5.4 SAFETY DURING MAINTENANCE

5.4.1 Piping
5.4.2 Tanks, scrubbers and alike
5.4.3 Mobile equipment
5.5 RESTRICT ED ACCESS AREA

5. PLANTS SAFETY
5.1 INTRODUCTION
This section studies the operating conditions and limitations for the safe use of
potentially nocive products to be employed in the plant.
It also includes a series of regulations to help avoid or foresee accidents, as well as

the immediate steps to be taken in case of accident.
This information is complementary to those of the costumer, and it should be part of

the Company Safety Regulations Manual.
All operators should be familiar with these regulations, and supervisors will have
copies of them to be distributed and discussed with all operators. Only when these
regulations are well studied and understood the operators can begin to work in the
plant start-up.
Supervisors will continuously make sure that these regulations are strictly followed,
and that whenever needed the appropriate safety equipment is used.
5.2 AMMONIA
5.2.1 Generalities
At atmospheric pressure and room temperature, ammonia is a colourless gas, less

dense than air and of irritating smell. In fertilizer manufactures it is frequently used at
high pressure in a liquid state, which is more dangerous because of its high
expansion coefficient. Thus, when a pipe or tank is being filled and it becomes
hotter, it exerts a very high pressure that tends to open the safety valves, or even
break the lines, because of its vapour pressure increasing rapidly with the
temperature, e.g.:
-33 C Atmospheric pressure

0 C 3.3 kg/cm2 (g)
15 C 6.4 kg/cm2 (g)
40 C 14.8 kg/cm 2 (g)
If liquid ammonia leaks into the air, it will rapidly vaporise increasing its volume
enormously. In this way 1 kg of ammonia (which in the liquid state occupies about
1.6 litters in volume) will rapidly form 1400 litters of a very cold vapour that will tend
to cool everything down to -33 C, condensing the water vapour of the air in its
contact, and forming a white cloud (aerosol) more dense then air, that will descend
to the floor trying to freeze anything with humidity.
At atmospheric pressure, mixtures of ammonia in air in a proportion of 15.5-28% in

volume at room temperature, or 14-30% at 250 C, can be explosive if in contact
with open fire.
Ammonia reacts avidly with water to form ammonium hydroxide giving off heat. If in
presence of water, ammonia will corrode copper and its alloys.
Due to its intense smell and very irritating nature, there is no risk of a person
willingly remaining in an atmosphere dangerously contaminated with ammonia.
Its physiological effects depend on its concentration in the atmosphere and on the
length of the exposure. These effects are summarized in the following table:
CONCENTRATION MAX.PERMITTED
IN AIR (mg/Nm 3) EFFECT EXPOSURE TIME
40 Irritating smell Long exposure

easily detectable
80 Nasty smell 8 hours
400-700 Nose, throat & eye 1 hour

irritation
2000-3000 Convulsive cough, Can be fatal even

serious eye irritation in minutes
Over 5000 Respiratory spasm In a few

& Lethal asphyxia minutes
In case of direct skin contact with liquid ammonia in a leak, it will produce burns by
dehydration. The severity of the burns will depend on the length of contact and the
body surface affected. Moreover, direct skin contact will also produce freezing of the
affected area due to the heat absorbed in its vaporization at atmospheric pressure.
1) All installations should strictly comply with the prevailing Safety Regulation
Laws for high pressure installations.
2) Installation inspections should be carried out as often as required by law.
3) Specially trained operators should only operate the ammonia installation.

4) When repairing the ammonia circuits, they will be emptied and washed with
water in the places to work on, leaving the circuits open.
5) All leaks found in the circuit should be immediately repaired regardless of

how small they may seem.
6) Rutinary safety equipment should always be worn, and the emergency

equipment should be kept easily accessible.
7) In case of leaks or circuit draining, operaries should work opposite to the

direction of the blowing wind.
5.2.3 Safety equipment.
5.2.3.1 Ordinary use equipment
1) Rubber or leather gloves.
2) Safety goggles.
3) Anti-gas mask with ammonia cartridge. It should be kept near the working area
ready to be used in inspections or in the repair of small leaks, as well as for
getting into the granulator in case of inspection after a shut-down.
4) Adequate clothing.
5) Safety helmets.
5.2.3.2 Emergency equipment
1) Fast actioning safety showers and eye washing fountains. They should be
installed near the ammonia handling area (granulator, pipe reactor, preneutralizer
reactor, ammonia separator/vaporizer).
2) Tight rubber suit.
3) Autonomous breathing equipment.
4) First Aid kit.
5) Water point with hose in order to neutralize any leak.
6) Fire extinguisher.
5.2.4 First Aid
5.2.4.1 Ammonia inhalation
There is no treatment required in case of exposure for a limited period of time to air
contaminated with small amounts of ammonia.
If the exposure has been in high ammonia levels and there is an oxygen device
available, this could be used by someone authorized by the doctor. If the accidented
operator is unable to breathe he should be resuscitated and a doctor immediately
called out.
Never give anything to an unconscious operator, or even if being conscious, without

the doctor's permission.
5.2.4.2 Ammonia ingestion
If someone has swallowed any ammonia and remains conscious he should be given
large amounts of water to drink in order to dilute the swallowed ammonia. If he is
unconscious nothing should be done without the doctor's permission.
Nothing should be done to make the accidented person vomit, but, if he

spontaneously did it, he should be placed face down and with his head low to
prevent any vomit getting inside the lungs and producing more damage.
5.2.4.3 Skin contact
As already mentioned, direct contact of ammonia with the skin produces burns by
dehydration and freezing. It is therefore extremely important to remove the
accidented person from the ammonia contact.
The accidented operator should be taken to the emergency shower, and once in the
shower he will be stripped off his clothing. He should be washed with plenty of
water and for no less than 15 min. Later he should be taken to a doctor for the
treatment of his burns.
Under no circumstances should oil or any ointment be applied over the affected
body surface during the 24 hours following the accident.
5.2.4.4 Eye contact
If any ammonia, no matter how little, has got in contact with the eyes, they should be
washed in the eye washing fountains with abundant water and keeping the eyelids
open, for a minimum of 15 minutes.
A doctor should be called out immediately and if, after a first 15 minutes washing,
the doctor has not yet arrived, keep washing for another 15 minutes.
After the second washing it will be applied in each eye 2-3 drops of a 0.5% solution
of pentocaine or any other aqueous anaesthetic. Never apply any oil or ointment
unless prescribed by the doctor upon examination of the patient.
5.2.5 Working in an ammonia atmosphere
Any person needing to enter an area whose atmosphere contains or may contain
significant amounts of ammonia, should be wearing the appropriate safety
equipment including helmet, goggles, anti-gas mask and gloves. He also should be
aware of the nearest safety showers and eye washing fountains location.
5.2.6 Ammonia Leaks
5.2.6.1 Detection
One way of by certain detecting an ammonia leak, is by using an open bottle

containing hydrochloric acid. Its vapours in the presence of ammonia vapours will
form a white cloud of ammonium chloride.
It is also possible to use a cotton impregnated with phenolphthalein solution which,

in presence of ammonia, will change its colour to red-pink.
5.2.6.2 Repairing
No leak will be repaired as long as there is any pressure left in the line.
No cut, welding, etc., will be made until there is the certainty that the system is
completely emptied of ammonia (there is no ammonia left in the system).
At the same time, care should be taken to keep all open flames, lighters, electric
sparks, etc. away from the ammonia containing atmosphere, bearing in mind the
explosion limits already mentioned.
5.3 PHOSPHORIC AND SULPHURIC ACIDS
5.3.1 Generalities
As any medium or high strength acid, phosphoric and sulphuric acids can produce
burns by dehydration and even carbonisation.
Logically, the degree of damage caused will depend on the acid concentration and
temperature and in the length of contact.
In DAP/NP/NPK manufacture the working acid concentrations are medium or high,

and the temperature varies from room temperature to 90 C. These conditions are
enough to produce serious burns unless preventive measures are taken.
5.3.2 Safety Regulations
1) All installations should strictly comply with the prevailing Safety Regulation
Laws for the use of strong acids at high concentrations.
2) All acid circuits should be properly signalled.
3) Periodic inspections of all circuit pathways should be made for the early
detection of any leak.
4) Any phosphoric acid leak found will be properly signalled until it is repaired. In
case of a large leak it should be repaired immediately. If the leak is of sulphuric acid,
it should be preferably repaired as soon as possible.
5) Never repair any circuit without first making sure that it is empty, washed and
pressureless.
6) Safety equipment should be worn when working with acid or repairing any leak.
5.3.3 Safety Equipment
1) Safety goggles.
2) Rubber gloves for reparations, and rubber or leather gloves for ordinary
operation.
3) Anti-acid suit.
4) Rubber or reinforced leather boots.
5) Fast actioning showers and eye washing fountains. These showers are the
same as the one needed for ammonia, although additional ones are required in
the scrubbing area.
6) Safety helmet.
5.3.4 First Aid
In case of any contact with phosphoric or sulphuric acid, the affected area, whether
the eyes or any other body surface, should immediately be washed with abundant
water, remembering that the seriousness of the burns will also depend on how
quickly we act and how long the washing takes.
After a first 10 minutes washing with water, and while waiting for the doctor, there
could be a second 10 minutes washing with bicarbonated water.
In case of eye contact with acid, after washing the eyes with water, some sedative
antiseptic solution drops could be applied.
Nothing else should be done until the patient is examined by the doctor.
5.4 SAFETY DURING MAINTENANCE
5.4.1 Piping
Before starting any pipe maintenance such as joints replacements, valves, etc. all
pipe ends should be closed with a blind flange to prevent any dangerous substance
accidentally getting inside.
As a rule the line will be completely drained and then washed with water to ensure
that there are not any product remains (never trust a closed valve). In any case each
pipe will be cleaned according to the nature of its content. Operaries should be
safely protected against any possible aggressive product projections.
In case of purge pipes, it should be ensured that they vent to safe areas. No welding
or cutting should be made without these precautions.
Ammonia gas and air mixtures can be explosive. It is therefore important that,
whenever there is a job to be done in pipes or tanks which may contain ammonia, a
special permission to do the job should be given after checking all safety measures
to be taken. This permission should be signed by the plant foreman or someone with
his authorization.
It also should be decided the required safety equipment (anti-gas masks, eye and
Skin protectors, water hoses, etc).
5.4.2 Inside tanks, reactors , scrubbers and alike
Tanks, reactors, scrubbers, etc., will be emptied and washed. Before getting inside a
permission for the job to be done will be obtained as indicated in the previous
section. Provisions should be made for the possibility of an explosive atmosphere,

toxic vapours, lack of oxygen, etc.
Blind flanges should be put wherever there is a possibility of gases, vapours or

liquids getting inside the tank, reactor.... Man holes will be opened to aerate the
tanks and fans will be kept on with the off switch sealed.
Fresh air masks should be used in case of lack of ventilation.
Electric equipment (e.g. agitators) fuses will be disconnected, and all vapour pipes
blocked.
All the time that a person is working inside there will be another person outside,
close to the man holes, in case of emergency.
5.4.3 Mobile equipment
All mobile equipment, conveyor belts, chains, motor driven belts, crushers, screens,
motors, drums, etc. should have all the required protectors to avoid accidents. All
safety measures should be checked before turning any mobile equipment on, taking
care about the maintenance or cleaning operations that could be on course. Never
touch or adjust any equipment while in motion.
During maintenance, equipment fuses will be disconnected.
5.5 RESTRICTED ACCESS AREAS
Pipe Reactor, Preneutralizer reactor, Ammonia separator/vaporizer and Scrubber

acid feeding areas, are potentially dangerous areas due to the chemical substances
used in them. As a rule these areas are restricted to plant and maintenance
operators only. The later should wear all protective clothing required when working
in those areas.
CHAPTER 6.- DAP & NPK MANUFACTURE

INDEX
6.1 PLANT CAPACITY

6.2 PRODUCT SPECIFICATIONS
6.3 RAW MATERIALS AND UTILITIES CONSUMPTION
6.4 PROCESS
6.4.1 Chemistry of the process
6.4.2 Basis of the process
6.5 PLANT START-UP OPERATIONS
6.5.1 Plant preparation operations
6.5.1.1 Filling the scrubbing section and pipe reactor vessel
6.5.1.2 Loading the Preneutralizer
6.5.1.3 Starting the main fans
6.5.1.4 Loading the initial recycle and the solid raw material bins
6.5.1.5 Ammonia feeding to plant and to Preneutralizer
6.5.2 Plant start-up
6.6 NORMAL PLANT OPERATION. POTENTIAL OPERATIVE PROBLEMS
6.6.1 Normal plant operation. Parameters control
6.6.1.1 Process flows for liquid section and scrubber control for DAP
NP and most NPK.
6.6.1.2 Process flows for solid section.
6.6.1.3 General considerations upon the common operative variables
relative to scrubbing liquids
6.6.1.4 Reaction section
6.6.1.5 Granulation loop equipment
6.6.1.6 Dedusting and gas scrubbing
6.6.1.7 Commercial product treatment until plant outlet
6.6.1.8 Other equipment
6.6.1.9 Adjusting the product grade
6.6.2 Operative problems analysis and correction
6.6.2.3 Scrubbing liquids
6.6.2.4 Granulator
6.6.2.5 Other general preventive measures
6.7 PLANT SHUT -DOWN PROCEDURE
6.7.1 Plant scheduled shut-down
6.7.1.1 Ordinary scheduled shut-down
6.7.1.2 Long-term scheduled shut-down
6.7.1.3 Annual plant shut-down
6.7.2 Plant emergency shut-down
6.7.3 Plant shut-down due to electrical power failure
6.8 CHANGE IN PRODUCT MANUFACTURE
6 DAP and NPK MANUFACTURE
6.1 PLANT CAPACITY
The plant has been revamped with the main aim to produce several NP/NPK/DAP
grades without disturbing actual production of TSP. The plant will be able to produce
NP/NPK with different sources of ammonia, as ammonium sulphate, urea or liquid
ammonia giving still more flexibility to the plant.
See below in table the different grades and production target of this plant
modernization.
Product Production (t/h)

Guaranteed Expected
23.10.10 1140 1191.3
15.15.15 1520 1567.5
DAP 1250 1300
20.10.10 1140 1187.5
MAP 1615 1710
13.13.17.2 1520 1567.5
Other NPKs 1140-1615 1187.5-2000
15.15.15 (H2SO4) 1320 1375

16.20.0 (H2SO4) 1400 1450
Plant capacity will be calculated, according on the grade and based on 22 working
hours/day, with allowance of 2 hours/day for cleanings and adjustments:
The foreseen recycle ratio, that is, the amount of recycled product per ton of
manufactured product, is 3.0:1 minimum and 4.5:1 maximum.
6.2 PRODUCT SPECIFICATIONS
The products DAP and 15-15-15 via sulphuric acid have been considered as the
basic ones for this operating manual, although may other product can be
manufactured in the revamped plant.
The product will comply with the following specification:

NPK 23.10.10 15.15.15 DAP MAP OTHER

NPK
Total N (%) 23 ? 0.9 15 ? 0.9 18 ? 0.5 11 ? 0.5 ? 0.5
Total P2O5 (%) 10 ? 0.9 15 ? 0.9 46 ? 0.5 52 ? 0.5 ? 0.5
W.S. P 2O 5 (%) 8 ? 0.9 13 ? 0.9 40 ? 0.5 45 ? 0.5 ? 0.5
K2O (%) 10 ? 0.9 15 ? 0.9
Moisture (% max) 1-1.5 1-1.5 1-1.5 1-1.5 1-1.5
Particle size:
(1-4 mm, % min) 90 90 90 90 90
(2-4 mm, % min) 85 80 85 85 80-85
Hardness:
(kg/cm 2 min) 1.5 2.5 3.0 2.5 1.5-3
6.3 RAW MATERIALS AND UTILITIES CONSUMPTION
For every considered product to be manufactured the specific raw materials and
main utilities consumption are the following (per ton of product):
Items 23-10-10 23-10-10 15-15-15 15-15-15 (H2SO4) DAP (alt. 1)

Ammonia (kg) 59-62 59-62 82-85 175-180 222-226
Urea (kg) 262-265 402-406 36-38 15-16 0
Amm.Sulphate (kg) 307-308 0 328-331 0 0
P2O5 (100%) (kg) 103-104 103-104 153-154 153-154 464-469
Sulph. acid (kg) 50 50 60 316-320 30
KCl (kg) 169-171 169-171 252-255 252-255 0
Filler (kg) 0 164 0 0 30
Kieserite (kg) 0 0 0 0 0
Electrical (kWh) 62.7-67 62-67 52-56 64-69 64-69
Water, (m3) 0.1-0.15 0.1-0.15 0.15-0.2 0.4-0.5 0.3-0.35
Steam, (t) 25-29 25-29 20-27 60-65 40-48
Fuel Oil (kg) 6.5-7 6-7 8-8.5 4.5-6 7-7.5
Items DAP (alt.2) 20-10-10 MAP 13-13-17-2

Ammonia (kg) 202-207 60-62 136-139 72-75
Urea (kg) 0 333-337 0 36-37
Amm.Sulphate (kg) 74 0 0 271
P2O5 (100%) (kg) 464-469 103-104 525-530 133-134
Sulph. acid (kg) 0 51 0 51
KCl (kg) 0 169-171 0 286-289
Filler (kg) 0 233 46 0
Kieserite (kg) 0 0 0 80-81
Electrical (kWh) 64-69 62-67 47-51 88-89
3
Water, (m ) 0.3-0.35 0.1-0.15 0.3-0.37 0.13-0.17
Steam, (t) 40-48 25-29 26-31 20-27
Fuel Oil (kg) 7-7.5 6.5-7 7-7.5 8-8.5
6.4 PROCESS
6.4.1 Chemistry of the process
During the manufacture of the DAP and the different grades of NP and NPK, the
main reactions will take place between the ammonia and the acids according to the
following equations:
a) With sulphuric acid

a-1) NH3 (gas) + H2SO4 ---------------> (NH4)2SO4 + Q1A
a-2) NH3 (liq.) + H2SO4 ---------------> (NH4)2SO4 + Q1B
b) With phosphoric acid

b-1) NH3 (gas) + H3PO4 --------------> NH4 H2PO4 + Q2A
b-2) NH3 (liq.) + H3PO4 --------------> NH4H2PO4 + Q2B
b-3) NH3 (gas) + NH4 H2PO4 ---------> (NH4)2HPO4 + Q3A
b-4) NH3 (liq.) + NH4 H2PO4 ---------> (NH4)2HPO4 + Q3B
The released heat, slightly dependent on the temperature, is around the following
values:
Q1A = 1800 kcal/kg NH3 gas

Q1B = 1500 kcal/kg NH3 liquid
The reaction (a-1) mainly takes place in preneutralizer, when producing ammonium
sulphate/phosphate and slurry, and also in the scrubbing section, whereas the
reaction (a-2) in the granulator solids bed, when sulphuric acid is directly fed to it.
Those reactions have priority over all the other reactions.
The reaction (b-1) will take place mainly in the scrubbing section, where the
phosphoric acid is always used as a washing liquid, to recover ammonia losses.
The reaction (b-2) will take place mainly in the pipe reactor, and in the preneutralizer
in some cases.
The reaction (b-3) will take place, whereas the reaction (b-4) always takes place in
the pipe reactor, preneutralizer and also in the granulator solids bed when acid
slurries with N/P molar ratio of 1.0-1.5 are ammoniated with liquid ammonia.
Other reactions can take place at the same time at the main reaction or during the
residential time in other equipment:
- Some ammonia will react with the impurities contained in the crude phosphoric
acid, coming from the phosphatic rock, such as iron, aluminum, magnesium,
calcium, fluorine, etc. producing a series of phosphatic complex compounds
such as:
Fe.NH 4(HPO4)2
Fe.NH 4 PO4.nH2O
Mg.NH4 PO4.H2O
Ca(NH4) 2 (HPO4)2.H2O
Al.NH 4PO4.F.H2O
- The main ammonium salts formed can react between the calcium sulphate
(present in the phosphate material anf filler) and the fed potassium chloride:
CaSO4+(NH4)2HPO4 ---> (NH4)2SO4 + CaHPO4

2KCl + (NH4)2SO4 ---> K2SO4 + 2NH4Cl
When gypsum is used as a filler is advisable to take care with the granulation pH
control, because high values of this parameter (over 7,0) means the conversion of
P2O5 (totally or partially) in tricalcium phosphate according to the following equation:
2CaHPO4 + CaSO4 + 2NH3 -> Ca3(PO4)2 + (NH4)2SO4
When this reaction occurs the available P2O5 decreases, with the consequent
economical and/or agronomic losses.
When the river sand or clay are used as a filler, is advisable to take care with its
calcium carbonate content, because high values of this can increase the sulphuric
acid consumption, in order to avoid ammonia losses and can reduce the water
soluble P2O5 in the final product, according to the following equations:
CaCO3+(NH4)2HPO4 ---> (NH 4)2CO3+ CaHPO4

(NH4)2CO3+ Q ------------> CO 2+ H2O+ NH3 (gas)
Some times, this reaction can occur in the stores. If this happens some ammonia
will escape from the granules and they will became wet and soft, producing dust and
caking.
For both reasons (acid consumption and product quality) is strongly recommended
to use any filler with a minimum content of carbonates.
One of the main physical parameters to consider in fertilizers granulation is the

amount of water entering the granulator. It will be basically determined by the
humidity of the ammonium phosphate or ammonium phosphate/sulphate slurries fed
from the pipe reactor and preneutralizer and the water content in the solid raw
materials fed to the granulator.
In all fertilizer granulation process there are, for each product and depending on the
raw materials used, most suitable pairs of temperature: humidity values in order to
obtain a good granulation yield, that is, obtaining the maximum of granules with the
desired granulometry.
The humidity and temperature of the product bed inside the granulator will
determine the system's "liquid phase" composed of the water and the solutions
formed depending on the solubility of the existing raw materials at that temperature.
This liquid phase will be balanced by a solid phase composed of the solid raw
materials and the recycled product.
There is an important direct ammonisation of the solids bed inside the granulator,
that will bring additional heat to the system. On the other hand, there will also be
some water vaporization from the solids bed, reducing its humidity, absorbing heat
from it and tending to cool it down.
A suitable liquid/solid phase ratio should be achieved inside the granulator in order
to obtain, at the resulting temperature and humidity, the maximum amount of
product with the desired specifications.
An excess of liquid phase could be directly due to an increase in the amount of

water provided through the solids raw materials and slurries, or to an increase in the
temperature that, on incorporating more free salts, will increase the liquid phase.
This heat excess could come from the sensible heat provided by the raw materials
and/or slurries, or by the reaction in the granulator solids bed itself. Also, a deficient
water evaporation in the solids bed will entail a liquid phase increase due to two
reasons: an increase in the solids bed humidity, and a temperature increase as
there is no heat dissipated in the evaporation. This could result in a product
overgranulation. Conversely, a liquid phase decrease would result in too many fines.
6.4.2 Basis of the process
The simultaneous use of a INCRO pipe reactor (PR) with the revamped
conventional preneutralizer (PN) and the ammonisation system in the granulator for
DAP/NP manufacture, or the use of first and last items (without PN) for NPK
manufacture, gives the system a great operational flexibility, making possible lower
recycles compared to the frequently used in the others slurry process without PR,
and, therefore, achieving higher production capacities by operating with the
minimum liquid phase required for a good granulation. The presence of the PR and
its capability to operate with ammonium phosphate slurries with very low water
content (if needed), promotes the system to obtain even lower recycles and higher
production capacities.
The totally conventional process (PN) produces ammonium phosphate slurries in

the conventional preneutralizer, from where they are transferred, by pumping, to the
granulator drum. This transfer, in order to be carried out without problems, requires
a minimum slurry water content which is higher than PR slurry need. In this
condition, liquid phase in the granulator increases and, in consequence, also the
recycle ratio tends to increase, limiting the plant production capacity.
On the other side, the totally PR process tends to be limited for heat balance
reasons, which can also imply higher recycle ratios.
Because of this, the use of a mixed process PN & PR present great advantages
when the proportion of slurry in the formula is very high (DAP, NP or NPK grades
with high amount of sulphuric in its composition). In case of producing grades with
less slurry content, the use of a single PR process is more advantageous than PN or
mixed PN & PR process, due to its simplicity and higher production performances,
since no heat limitations are present.
Inside the P.R. the ammonia becomes in contact with the phosphoric liquor (mixture
of crude phosphoric acid and liquids from the gas scrubbing section) in a high
efficiency reaction head. The neutralization reaction continues and ends inside the
slurry distribution pipe that discharges the slurry inside the granulator, directly over
the solids bed. The high efficiency of the mixing head and the short residential time
of the slurry in the distribution pipe, as well as the self-cleaning effect due to the high
speed of the steam generated inside this pipe, makes possible to work with very low
moisture, if necessary for the process, or, in case of increasing production capacity
by using more concentrated phosacid.
In all cases of DAP/NP/NPK production, using or not sulphuric acid in its

composition, phosphoric acid is used as washing liquid in the scrubbing system
(except in tail gas scrubber where process water is used together with small
quantities of sulphuric acid).
The recommended parameter are to use more diluted phosacid for second step of
scrubbing (scrubber vessel), in order to minimize fluorine stripping, and more
concentrated phosacid for first step of scrubbing (pre-scrubber vessel). This
phosacid concentration must be as low as possible and the total amount of P2O5 fed
to the scrubber system has to be carefully studied to obtain a liquor with N/P molar
ratio of about 0.3-0.6. Lower values can help fluorine stripping and higher values
can cause problems of insolubility. Producing NP or even NPK grades with high
amount of sulphuric acid and ammonia contents, part of this sulphuric acid (15-25%
of the total) will be fed to the first scrubbing step together with the phosacid.
In case of NPK production using single PR process, the washing system phosacid
liquor, partially ammoniated, is sent to the pipe reactor via pipe reactor vessel,
where it is mixed with the remaining strong phosacid not fed to the scrubbing
system. Pipe Reactor will produce ammonium phosphate slurry with N/P molar ratio
of 1.35-1.5, although this value can be ranged, if necessary, between 1.0 and 1.8
according phosacid concentration.
In case of DAP production, using mixed PN & PR process, the partially ammoniated
liquor, is divided in two flows: one of them is sent to the pipe reactor via pipe reactor
vessel, where, after being used as a washing liquid, it is mixed with the remaining
strong phosacid as in the previous case and the rest is sent to the preneutralizer,
where ammonium phosphate slurry will be produced with N/P molar ratio of 1.4-1.5 .
Pipe Reactor will work producing the same type of slurry as in case of NPK
production.
In case of producing NP or NPK grades with high sulphuric acid content in its
composition, which means the use of a mixed PN & PR process, the preneutralizer
will work producing ammonium sulphate/ phosphate slurry. Final proportion between
both salts will dependent, logically, on the N-P of the grade. Washing liquid is also
divided in two flows as in case of DAP production. To the preneutralizer is also fed
most of the sulphuric of the formula . Usually sulphuric acid is neutralized in the PN
to a N/S molar ratio of 1.7-1.8, without arriving to N/S ratio 2.0 to avoid
crystallization problems into the reactor. Compatible with that N/S ratio, the
ammonisation of the phosphoric acid has to be carried out in the preneutralizer to a
N/P molar ratio of about 0.8-0.9 maximum. It is recommended not to exceed this last
value in order to avoid crystallization problems which can arrive to plug the slurry
transfer line, the distribution tube and also the preneutralizer itself. Meanwhile, Pipe
Reactor will work producing the same type of slurry as in case of DAP and NPK
production.
6.5 PLANT START-UP OPERATIONS
6.5.1 Plant preparation operations
Once all the operations previous to the plant start-up indicated in section 3.1 are
performed, having completed the washing and calibration of the appropriate
instruments, the operations for the future manufacture of the desired products can
be started, such as the tanks filling and starting the different equipment.
Thus, starting with the completely empty plant, with all the valves closed, the
operations for the initial loading of the installation are the following:
6.5.1.1 Filling the scrubbing section and pipe reactor vessels
After having filled all vessels with water, all this should be drained and cleaned. The
filling must be done, according to the formula to be manufactured, as follows:
% (in volume) DAP 15-15-15

12-D-311 Tail gas scrubber
Water 100 100
02-D-310 Dust scrubber seal tank
Water 80-85 94 - 96
Phosphoric acid (48%) 15-20 4-6
02-TK-302 Scrubber seal tank
Water 45-50 78 82
Phosphoric acid (48%) 50-55 18 22
12-D-311A/B Granulator pre-scrubber
Water 15 20 60 65
Phosphoric acid 80 85 35 40
12-TK-301 Pipe reactor vessel
Water 10 - 15 10 - 15
Phosphoric acid 85 90 85 90
The reservoir of 12-D-312 Tail Gas Scrubber will be fed with process water by
opening the manual valves at the existing head line. LCV (existing) will close
automatically when the working level is reached in 12-D-312. At this time, open the
manual valves of the washing lines and start the pump 12-P-313A/B/C/D. The
transfer line 80-WAS-E5-a-108 must be kept closed during this operation.
After this operation manual valves of sulphuric acid line to 12-D-312, 20-SA-B1-106,
coming from battery limit must be opened and the pH adjusted with AIC-301. ACV-
301 will close automatically when the pre-fixed pH level in AIC-301 is reached in
bottom of 12-D-312.
For the time being, no sulphuric acid will be added, waiting till the moment when
ammonia is arriving with incoming gases.
The Scrubber Vessels (02-TK-302/02-TK-310) filling has to be done following the

next instructions:
a) With the phosacid supplying pumps in operation, open the manual and control
valves of the line 40-PA-E5-a-104/DN50 existing line) from the battery limit to
the 02-TK-302/02-TK-310 Scrubber Vessels, filling the vessel till a value which
is the desired level (typically 60%) multiplied by the percentage of phosacid
feeding in volumne, as expressed in previous table for different grades, as
indicated in LIC-305/existing. Close Phosacid control valve.
When the level in 02-TK-302/02-TK-310 reaches about 50%, start the agitators.
b) Open the valves of the correspondent transfer line 80-WAS-E5-a-108/existing

from Tail Gas Scrubber to Scrubber Vessel 02-TK-310/02-TK-302 and set the
LIC-302/existing in automatic mode 60% set point to fed water according given
instructions at the beginning of 6.5.1.1. Water make-up will be controlled by
LCV-302/existing connected to LIC-302/existing.
c) Open the manual valves of the washing lines to 02-D-301A/B, 02-D-302A/B and
02-D-310A/B and those on selected pump suction line. Start the pumps 02-P-
311A/B // 02-P-304A/B 02-P-305A/B. The transfer lines 80-WP-E5-a-
109/existing must remain closed. Check the density of the acid in 02-TK-
310/02-TK-302. It should be around 1000-1150/1150-1250 depending on the
grade 15-15-15 or 18-46-0, which roughly corresponds to expected P2O5 and
water content in each case. Adjust with acid or transfer water flow if necessary.
Add some defoamer if required.
d) In parallel with 02-TK-302/02-TK-310 filling, 12-D-311A/B Granulator Pre-

Scrubber can be also filled up. All valves in phosacid line 80-PA-E5-a-103
should be opened. For each flow the set must be fixed in their corresponding
flowmeter to fill the vessel till 60% level indication in LIC-304. Sulphuric acid can
be fed just after starting production, according to production rate given flow to
avoid free sulphuric acid in the washing liquid.
e) Once the 60% level is reached in 12-D-311A/B, open the manual valves of the
washing lines to 12-D-311A/B (recirculation) and the pump suction line, starting
the selected pump 12-P-312 A or B. The transfer lines 100-WP-C3-b-105 to
pipe reactor vessel, 100-WP-C3-b-106 to preneutralizer and 50-WP-C3-b-121
to granulator, must remain closed. Add some defoamer if required.
f) Check the density of the acid in Granulator Prescrubber. It should be around

1.35-1.45 for 15-15-15 and around 1.4-1.5 for DAP. Adjust with phosacid or
water if required. Set LIC-304 in automatic mode at 60% set point and open the
transfer line from scrubber vessel 02-TK-302.
g) Pipe Reactor vessel 12-TK-301 should be also filled. Add phosphoric acid and
process water alternatively, according the proportions in volume given for this
item at the beginning of 6.5.1.1, by opening line 50-PA-E5-a-102 and 40-PRW-
A2-a-103 valves respectively , till 50% level (LIC-301).
h) When the level in 12-TK-301 reaches about 50%, start the agitator 12-M-365.
i) Check the density of the acid. It should be around 1.55-1.6 for all DAP/ NP /
NPK grades, to start the process. Adjust with acid or water if necessary.
Add some defoamer if required. Set LIC-301 in automatic mode at the final set point
after adjusting acid concentration (between 50-60%).
At this point, all the vessels are filled at their working levels and all the scrubbers are
being fed with their correspondent washing liquids.
Sulphuric acid will not be added till the moment the operation is started and a
considerable amount of ammonia is arriving to the scrubber, to avoid any corrosion
problems.
6.5.1.2 Loading the Preneutralizer
When mixed process, PN & PR, is going to be used, what happen for the production
of DAP or 15-15-15 (SAB), the preneutralizer has to be loaded with the
correspondent slurry before starting the normal production.
The preneutralizer will be loaded in two steps, and the load depends if product to be
manufactured is DAP (without sulphuric acid to PN) or 15-15-15 (with a lot of
sulphuric acid to PN).
In the first step, the preneutralizer will be initially loaded with the required amount of
phosphoric acid at the same concentrations given for prescrubber vessel, and, in the
second step the loading is completed by the addition of liquid ammonia to n/P 1.4-
1.5 in case of DAP and 0.7-0.9 in case of 15-15-15 production. In all cases, second
step will be carried out after being started the main fans and the scrubbing system
pumps in order to recover most of ammonia escaped from the reaction. This second
step has to be carried out, logically, only if the production is nearly to be started;
otherwise the obtained slurry should be kept too much time in the preneutralizer.
When producing SAB grades, there will be a third step constitutes on the
simultaneous addition of concentrated sulphuric acid and the required ammonia for
its neutralization.
In the first step, producing DAP , the preneutralizer will be initially load as follow :
- Phosacid of about 40-41% P2O5 will be load by feeding phosacid and water, until
reaching around 50% level in the preneutralizer.
- Take note of the total fed acid, in the totalizer FQ-341, in order to calculate the
necessary ammonia for the first slurry loading. During this operation, all manual
valves of liquid ammonia to preneutralizer while slurry valves have to remain closed.
- When the level in the preneutralizer reaches around 50% and the feeding of acid is
finished, start the agitator 12-M-356, take a sample of acid and check density. It
must be around 1.48-1.52 at ambient temperature. Adjust density, if necessary by
feeding more phosacid or water.
In the first step, producing 15-15-15, the preneutralizer will be initially loaded as
follows:
- Phosacid of about 14-15% P2O5 will be load by feeding phosacid, through FIC-341,
and process water, until reaching around 40% level in the preneutralizer.
- Take note of the total fed acid, in the totalizer FQ-341, in order to calculate the
necessary ammonia for the first slurry loading. During this operation, all manual
valves of liquid and gas ammonia to preneutralizer and slurry valves have to remain
closed.
- When the level in the preneutralizer reaches around 40% and the feeding of acid
and water is finished, start the agitator 12-M-356, take a sample of mixed acids and
check density. It must be around 1.1 at ambient temperature. Adjust density, if
necessary by feeding more water or phosacid.
In this first step of loading, no sulphuric acid will be added to preneutralizer, to avoid
corrosion risk. Sulphuric acid will be added together with the liquid ammonia, in the
last loading step, to produce the initial slurry.
6.5.1.3 Starting the main fans
Once filled the scrubbing system vessels and after keeping the recirculation pumps
on, sending liquid to the spraying points, the fans will be started, always before
feeding ammonito to PN.
The fans will not be started without at least one of the corresponding scrubbing
recirculation pumps being in operation, and its respective damper closed. This will
avoid any damage to the fan motor and the product accumulation inside the
scrubbers.
With the dampers initially closed, the Granulator Scrubber Fan 12-C-301, the Dryer
Scrubber Fan 12-C-302 and the Dust Scrubber Fan 12-C-310, will be started. Once
they reach their nominal velocity, their corresponding dampers will be opened until
PDIs show the normal expected pressure drop, checking that the power
consumption readings in their respective ammeters is normal.
These fans, are big devices with a limited number of starts per hour. This, according
to the interlocking system, makes it very important to start them with the damper
closed, to avoid overloading the motor.
With the scrubbing system in operation, it will be checked again that there are not
liquid leaks and that the scrubbing liquids flow freely through all the towers and duct
washing spraying nozzles. The approximate flows to be kept to the scrubbers are
the ones indicated by the equipment suppliers for design conditions.
6.5.1.4 Loading the initial recycle and the solid raw materials bins.
Before beginning with the start-up procedure and in order to avoid slurry pasting
problems inside the granulator, the plant should be provided with the required
amount of recycled product, with the same or similar composition than the grade to
be manufactured.
There should be enough fertilizer in stores to load the recycle system, for which
about 120-150 ton of granulated DAP and 100-120 ton of the granulated NPK to be
produced are required.
For the first start-up there should be available DAP, NP or NPK of the same quality
and grade than the one to be manufactured. Otherwise the initial start-up could take
an unnecessarily long transitory and correction time, which is not so convenient, at
least until the operators get enough experience with the new process. In subsequent
manufactures, the final product could be used to load the recycle, or even the
recycle extracted from the installation from previous DAP/NP/NPK manufactures
due to a formulation change.
This initial load will be introduced in the unit, controlling its weight, through the raw
material bins which were emptied at that time. Before feeding any product, the
granulation loop equipment, composed of the following elements, should have been
started:
a) Granulator
b) Granulator elevator
c) New Recycle belt conveyor
d) Recycle drag conveyor
e) Screen product conveyor
f) Process Screens
g) Product drag conveyor
h) Oversize mills
i) Dryer exit elevator
j) Dryer and dryer lumps crusher
When all that equipment has been started, and after bins are filled with the
corresponding seed material, start the product feeders 12-G-314 (i.g) and keep it in
operation feeding seed material till having the desired throughput in 12-WQ-327
(throughput weigher).
The granulation loop could be started automatically, as indicated in Section 2.3, or

manually, following the same sequence of steps than the automatic. (The equipment
supplier Technical Manual should be consulted for any specific procedure to follow
on starting the equipment).
The Dust Scrubber fan 12-C-310; 12-C-301 and 12-C-302 must remain working
when the plant is filled with granulated seed, due to the dust produced during the
filling operation. The dampers, however, should not be too open.
Similarly, the granulator's air suction should be tried to be done from the product exit
side in order to not to suck air from inside of the drum and avoid a lot of dust going
to the scrubbing, which could increase the acid N/P inside it, as the scrubbing liquid
would not be spent. This will be done by fully opening the doors in the granulator
product exist side.
Another preventive measure is to feed very small quantities of water/steam to the

granulator, to slightly wet solids bed. If this practice is followed it is recommended to
start burner at low capacity, to avoid product moisture increase.
The remaining not mentioned equipment (unless water is added to granulator) be

kept stopped, particularly the burner and the dryer combustion chamber fans, as
well as the on-size product exit section: recycle regulator belt conveyor to cooler,
polishing screen, etc., until its dispatch to stores.
With all this, the system will work in a closed circuit, till achieving the required
system load to begin production.
After some experience, besides the value indicated in the throughput weigher, just
by the readings of the recycle equipment ammeters, mainly elevator or dryer, it will
be possible to know the system's level of load.
Later, the remaining ammeters will be checked to ensure that the equipment is
working properly.
Also during this recirculation period, it will be checked that there are not any
abnormal liquid or dust leak, and that the flap valves at the bottom of the cyclones'
hoppers work properly.
If only one bin is used, meantime these operations are performed the raw material
weigher not used for the seed material will be filled with the required product. Once
recycle filling has been completed, the other bin will be filled with its corresponding
raw material, if required.
This initial raw materials filling will be done till reaching 30-50% of the total capacity
of each bin. Obviously, during this operation, the feeders must be stopped.
The operators will carry on this loading operation carefully, in order to avoid mixing
of different products in the bins. It will be checked that no product leaks are
produced from the raw material input equipment.
6.5.1.5 Ammonia feeding to plant and to Preneutralizer
Before starting this feed the safety checks indicated in Section 2.2.1 and 5.2 must
be completed, particularly, before letting the ammonia pass from stores to the plant
piping, it should be checked that all valves are closed, including the control valves
and all purging valves. To purge its corresponding section, each of these purging
valves will be connected to a flexible tube whose free end will be submerged in a
water containing bin. In this way, at the time of the purge, the ammonia will make
any air inside the line bubble through the water. When the bubbling stops, the
purging valve will be closed and the next section purged.
All the system, from battery limit to the different points of consumption, will be
conveniently purged of any air that might be inside. For this purpose, the automatic
valves will be changed to their "manual" mode. For the lines to the granulator and
pipe reactors the purge will be done towards the inside of the drum. The purging
time should be limited to 1-2 minutes maximum in order to avoid too much ammonia
going to the scrubbing system increasing the N/P of the acid circulating in a close
circuit inside it.
With the help of the corresponding valves, the liquid ammonia collector lines will be
filled with ammonia, keeping each distributor access valves to the preneutralizer
closed. Liquid ammonia line 50-NHL-L1-106-C will be used for this purpose. When
the system reaches its equilibrium pressure, the distributor valves will be completely
opened, letting the ammonia pass inside the preneutralizer via FCV-342, purging the
final sections to the PN inside. Second loading step will be made, from this point,
depending on the product to be manufactured, in the following way.
Slurry for DAP production:
a- Calculate total amount of P2O5 fed during the first loading step, from the
totalizer FTQ-341 data.
b- Calculate total amount of NH3 need to arrive to N/P molar ratio of 1.45 taking into
account the previous calculated P2O5.
c- Start the agitator
d- Feed liquid ammonia to the preneutralizer, through FIC-342, controlling the total
fed amount in the totalizer FTQ-341, until being fed all calculated amount.
e- Once most of the ammonia flow has been added, the molar ratio and the slurry
density will be checked and adjusted by adding more ammonia, more acid or
even more water (N/P ratio must be 1.4-1.5 and the density around 1500-1550).
f- During the operation the functioning of the agitator will be checked by observing
if there are any local flashes due to the lack of agitation, causing the freezing of
some areas at the bottom of the preneutralizer 02-R-303. Also abnormal noises,
vibrations and movements will be observed and checked.
Slurry for 15-15-15 production
a- Calculate total amount of P2O5 fed during the first loading step, from the totalizer
FTQ-341 data.
b- Calculate total amount of NH3 need to arrive to N/P molar ratio of 0.7 taking into
account the previous calculated P2O5.
c- Start the agitator
d- Feed liquid ammonia to the preneutralizer, through FIC-342, controlling the total
fed amount in the totalizer FTQ-342, until being fed all calculated amount. Check
N/P ratio and adjust if required.
e- From the total fed P2O5, calculate the necessary total amount of sulphuric acid to
be fed to the preneutralizer and the total amount of ammonia to neutralize this
sulphuric acid:
kg sulphuric 98% = kg P2O5 fed x 3.4

kg ammonia = kg sulphuric 98% to feed x 0.32
f- Calculate the corresponding flows in m 3/h for ammonia and sulphuric acid, which
must be proportional to the above calculated amounts. These flows will be feed
simultaneously to the preneutralizer through FIC-342 (ammonia) and FIC-343
(sulphuric acid).
g- Open manual valves in the sulphuric acid line 80-SA-B1-103 to PN and start
feeding of sulphuric and ammonia until being fed the above calculated total
amount of both reactants.
h- Once the ammonia and acid flow have stopped, the molar ratio and the slurry
density will be checked and adjusted by adding more ammonia, more acid
sulphuric or phosphoric, or even more water (N/P ratio must be 0.8-0.9 and the
density around 1550-1600).
i- During the operation the functioning of the agitator will be checked by observing
if there are any local flashes due to the lack of agitation , causing the freezing of
some areas at the bottom of the preneutralizer 02-R-303. Also abnormal noises,
vibrations and movements will be observed and checked.
In both cases, DAP and 15-15-15 slurries, the ammonia feeding will produce
reactions with the phosphoric and sulphuric acids and an increase in the slurry
temperature inside the preneutralizer. This temperature can be observed in TI-369
from DCS system and also from local TI-370, located on the wall of the
preneutralizer. If necessary, steam can be fed to the preneutralizer to ensure that
the slurry is hot enough in this step. (Temperature has to be normally around 110-
120C in case of ammonium phosphate slurry, and around 120-130C for
ammonium sulphate / phosphate slurry).
When the ammonia feeding stops, the steam will be automatically introduced to the
preneutralizer, commanded by PV-301. While all the remaining operations are
completed, before beginning production, the steam will be kept entering to the
preneutralizer, checking that the slurry temperature in TI-369 / TG-370 does not fall
below 100-105 C.
With the ammonia system totally purged and full from the storage until the control
valves, the plant is ready to start.
6.5.2 Plant start-up
Once the preliminary operations indicated in the previous section are completed, we
will have the plant full with recycle, the preneutralizer full of slurry (in case of mixed
process), the granulation loop working in a closed circuit, the scrubbing system and
pipe reactor feed vessels full, the pumps recirculating liquid to the scrubbers, being
fans also in operation.
Now is the time to do all the remaining steps required before the plant start-up, that
is, from the raw materials feeding, product exit and plant stabilisation, to the
dispatch of the nominal amount of product, of the desired specifications, to stores.
Table 6.5.2 shows all feeding / transfers flows for the production of grades DAP and
15-15-15.
The plant will be gradually started, beginning manufacturing only 70% of the nominal
capacity until the plant is stabilized with this production for 2-4 hours. Once the plant
is stabilized with these conditions, production will be gradually increased until the
foreseen nominal capacity for the product is reached. The swiftness with which this
nominal capacity is reached will depend on the plant performance and the operators
degree of control in using the new installation.
DAP/NP/NPK manufacture will be according to the following specifications:
Balancing the systems
The first thing to do is check that all scrubbers vessels are filled up to working level,
the acid concentration is the correct one and the recirculation pumps are on.
The levels in the tail gas scrubber , the scrubber seal tank, dust scrubber tank, the
granulator pre-scrubber and pipe reactor vessel, will be set on automatic mode,
opening the required manual valves on the transfer lines. As the level in the
reservoir of Tail Gas Scrubber decreases, process water will be automatically fed to
maintain the levels.
Scrubber liquor concentration should be closely monitored until it has been

established that the correct concentration is being obtained. The acid/water ratio
may be changed either by changing the quantities of phosacid or changing the
quantity of water advanced from TGS. Since the plant will be normally fed with a
constant acid fed, the scrubber acid concentration will be adjusted by changing the
rate of advanced water.
The exhaust fan dampers should have been gradually opened to bring them to
normal load capacity.
In the granulator the air entrance at the drum outlet side will be partially closed,
slightly opening the one at the solids inlet. The damper, located in the preneutralizer
fumes suction line should be about 80-85% open.
Phosphoric and sulphuric acid
The operator sets the overall flow of phosphoric and sulphuric acids according to the
rate of operation chosen.
The operator sets initially the split of phosphoric acid going to PR Vessel 12-TK-301,
Granulator Pre-Scrubber 12-D-311A/B, Scrubber Seal tank 02-TK-302 and Dust
scrubber seal tank 02-TK-310. The P2O5 will be splitted in the following way,
according the grade :
DAP 15-15-15
P2O5
To Granulator Pre-scrubber 65-75% 38-42%
To Pipe Reactor Vessel 16-20% 35-40%
To Scrubber Vessel 8-10% 15-20%
To dust scrubber seal tank 03% 3-5%
Sulphuric acid goes to the tail gas scrubber 12-D-312A/B, granulator pre-scrubber
12-D-311A/B, scrubber seal tank 02-TK-302, granulator 02-M-361 and
preneutralizer 02-R-303.
The flow of sulphuric acid to the tail gas scrubber is automatically adjusted via pH
meter, to maintain a pH of about 5 in this circuit, the optimum to recover ammonia
without evolving excessive fluorine.
Sulphuric acid addition to scrubber vessel must be done only occasionally if there is
any N/P ratio problem due to temporary anomaly in the pre-scrubber system.
Producing DAP and NPK products without high sulphuric acid content (when
preneutralizer produces only ammonium phosphate slurry or is stopped), the
remaining sulphuric acid, not used in the tail gas scrubber, must be always fed to
the granulator pre-scrubber 12-D-311A/B with the main objective of controlling N/P
ratio below 0.5 in its scrubbing liquid or to granulator.
When the preneutralizer has to produce ammonium sulphate/phosphate slurry,

which is the case of NPK 15-15-15 grade, with high sulphuric acid content, normal
split will be as follows:
15-15-15
To 02-R-303 (preneutralizer) 70-75%
To 12-D-312A/B (tail gas scrubber) 0.5-0.8%
To 02-M-361 (granulator) 2-4%

To 12-D-311A/B (Granulator pre-scrubber) 22-25% (Rest)
Primary scrubber solution
Enough process water, phosphoric acid and sulphuric acid must be used in the
scrubber system to maintain a mole ratio N/P far from the crystallization point, as
well as to provide a volume of liquid enough to contain the dust and ammonia
carried over.
This liquor is expected to be in the range of 38-41% P2O5 for DAP production, 11-
17-19% P2O5 for NPK production(15-15-15 grade) , for Granulator Pre-scrubber 12-
D-311A/B
Pipe reactor feed vessel
The bulk of the phosacid can be introduced through scrubbing system, but usually
when P2O5 quantity is large enough, as expected in our case, the operator will feed
some fresh phosacid to the pipe reactor tank 12-TK-301, via FIC-337, to provide the
rest of the P2O5 not processed through the scrubber system. After mixing with total
or part of the washing liquor coming from 12-D-311A/B (the other part is sent to the
preneutralizer when mixed process is used), the P2O5 content will be adjusted
around 41-43% in case of NPK production and around 44-46% in case of DAP or
NP production .
Pipe reactor feed
From 12-TK-301 phosacid acid liquor will be fed, in all cases, to the Pipe Reactor
12-R-301A/B, via FIC-338/339. To produce DAP two pipe reactors can be used and
in case of 15-15-15, only one PR plus the use of the PN.
To the same Pipe Reactors will go the required liquid ammonia, whose flows are
controlled by FIC-333/334.
HS-319/320 will interlock HV-301/302 (to open the steam inlet) with the ammonia
and phosphoric acid feeding valves (as well recirculating On/off valve in PR vessel
and drainage ON/Off valves in purge pot), which will be closed to allow for cleaning.
Switches will also have stand-by or operation position.
Process Water
The level control of vessels is achieved by cascade level control.

The level control in the bottom of tail gas scrubber 12-D-312 system is done
automatically by existing LIC with process raw water.
No additional water will be added to any scrubbing point, just to occasionally adjust
concentrations. Some times to change quickly the working conditions, process water
could be fed directly to the following equipment:
- To the pipe reactor vessel, through manual valve

- To the Granultor Pre scrubber, through FI-307
- To the preneutralizer.
For the same reason, water coming from 12-D-312 could be fed directly to the
granulator via FIC-352.
Prior to start any liquids addition for granulation, the granulation loop will be started,
beginning for the granulator and following the described normal sequence till
finishing for the dryer.
At the same time it will be checked that should the recirculation flows to the
scrubbers are well adjusted (they correspond to the design values calculated by the
supplier). Also, the scrubbers pressure drop will be checked.
Simultaneously with all these operations and 5-10 minutes before the first slurry
discharges to the granulator, the dryer burner will be started. For grades not
containing a lot of urea, which is normal situation, outlet temperature should be
monitored. Temperatures will be programmed between 120-150 C (200 C max)
and 90-100 C (105 C max) for inlet and outlet respectively, the range covering the
different formulas.
Next, the equipment for the product extraction from the granulation loop to stores
will be started, that is, the rotary cooler 02-M-363, the product elevator 02-M-308,
the polishing screen 12-F-302,coater drum 02-M-364 and the final product conveyor
02-M-401, as well as all transport equipment, out of B.L., from this last equipment to
the stores. The product feeder 02-D-326 will, however, be kept stopped until the
product is to be extracted from the granulation loop.
When everything is ready we start the addition of solid raw materials through the
required feeders.
Then we can start the transfer of slurry from preneutralizer to granulator but only in
case of 15-15-15 production which will be made using mixed PN & PR process. For
this purpose FIC-302 or 312 will be switched to the manual position until
approximately 40% of the FCV-302 or 312 is opened. The transfer pump chosen,
02-P-301A or B, will then be started and FIC-136 A or B switched back to automatic,
to the flow indicated in Table 6.5.2 according to the product and hourly production.
At the same time will begin the ammonia feed to the granulator through the
ammonia sparging system 12-R-302, via FIC-335. Before the ammonia feed the
spargers will have been steam flushed to ensure they are clean. During this step, as
the slurry coming from the pipe reactor is still not produced, ammonia feeding to
granulator has to be carefully managed to obtain semi-dry product in the granulator
solids bed, avoiding pasting and excessive dried material to reduce ammonia
losses. Product leaving granulator drum will be continuously observed and manually
checked during at least 10-15 min.
At the same time the following points will be checked:

- The slurry transfer line has the steam tracing in operation.
- The recirculation flows to the scrubbers and the scrubbers pressure drop.
Then we can start the pipe reactor with liquid ammonia and the corresponding acid
and feed the rest of liquid ammonia required for the granulation. Before the PR A
or B (or both in case of DAP production) is working, the liquid ammonia feed to the
granulator will be increased, via FIC-335, from its flow used to neutralise PN slurry
feeding. Previously to PR starts it has been steam flushed actioning HS-319/320 for
1-2 minutes.
Pipe reactor fed pump 12-P-315A/B will be used to feed phosacid liquor via FIC-
338/339, meanwhile liquid ammonia will be fed via FIC-333/334 depending on the
chosen pipe reactor.
If the ammonia and phosacid liquor feed to the PR were manually performed, and
although all will be started almost simultaneously, the ammonia feed should be
started first to avoid the acid being poured directly on to the solids bed which will
past it, mainly when mixed process is being used and slurry from preneutralizer feed
to the granulator.
At this point of the granulation process, the product leaving the granulator will be still
more carefully observed for at least 5-10 minutes to ensure that it is well dried and
that the ammonization is being properly carried out.
If all observed parameters are correct, we can start ammonia feeding to

preneutralizer, fresh acid feedings to all equipment according the flows given in
Table 6.5.2 and also the scrubbing liquid transfer from 12-D-311A/B to the
preneutralizer 02-R-303 and/or pipe reactor vessel 12-TK-301. Required flows must
be adjusted and the level in all vessels and preneutralizer controlled until the plant is
stabilized.
By observing the product, its moisture, granule size..., at the granulator exit, it will be
possible to know whether the amount of recycle used is adequate. If this is the case,
once all parameters are stabilized and the on-size product leaving the screens
complies with all specifications, the commercial product will start to be extracted by
the product feeder 02-D-326, which will control the product exit flow (indicated by
12-WQ-326) until it equals the flow of the raw materials entering the plant. The
product leaving to stores should normally have a temperature lower than 50-55 C,
after passing through rotary cooler and polishing screen. Only when cooler air chiller
is not used that temperature can arrive to 50-60 C.
The final product flow sent to the storage is shown and totalized in 02-M-401.
The successive increase of capacity till arriving to 100% will require to increase the
feed to the granulator of slurries coming from the PN and PR, or only from PR in
case of DAP production, being necessary to previously increase the amount of
recycle to the granulator, by decreasing the final product extraction. This will keep
liquid/solid ratio constant. Obviously, liquid and solid raw material feeding will be
proportionally increased as production capacity increases.
Under those circumstances, the conditions at the granulator exit will be observed
again, until the system stabilization with those new capacities. Once it is stable, the
commercial product extraction to stores will be increased again to the new
production rate, according to the new total raw materials feed.
During this phase, the recirculation flows to the scrubbers will be checked, as well
as their pressure drop which should be adjusted to the stipulated values.
Also during the phases when the capacity is increased the operational parameters
control, indicated in Chapter 4, will be done with the frequency that the plant start-up
performance requires.
With the plant stabilized and the balance between the nutrients entering the plant
with the raw materials and the ones leaving with the product, any eventual
instrument lack of accuracy will be easily detectable. The operational parameters
will be closely observed as well as the equipment mechanical and electrical
performance. Some adjustments may be necessary depending on the analysis
results, such as flow adjustments in order to change the molar ratios N/P in the
reaction section or granulator. Through the granulator suction doors, the pressure
inside them will be equilibrated in order to obtain adequate suction. The door on the
granulator product inlet side will be partially opened observing that there is not too
much dust taken to the exit duct.
In the preneutralizer 02-R-303 (if used) will be observed the double level indicator
LI-302 and LI-303 and the temperature in TI-369 / TI-370 (DCS/local), as well as the
feeding flows and the slurry transfer flow in order to detect any possible abnormality
from the foreseen parameters. But most important is to check the slurry condition by
analysing its density and its N/P molar ratio, to quickly determine if any corrective
action is needed. In this phase of the production, when the plant is just starting, is
very important to increase the frequency of analysis to adjust as soon as possible
the slurry quality, which will help in the plant stabilisation.
In the pipe reactor 12-R-301A/B will be observed the ammonia and phosphoric acid
pressures at its inlet, shown by PG-328/329 in local and PI-331/332 DCS
respectively, and the slurry distribution pipe temperature indicated by TI-366/TI-367.
Those pressures will be interconnected: if the acid pressures are continuously lower
than 2 kg/cm2 the slurry exit slots in the distributing tube will be partially closed (this
will be done shutting the plant down) by using the correspondent collars, in order to
increase that referred pressures, which will improve the mixing inside the distribution
pipe and the reaction chamber. Meanwhile, the ammonia pressure should be at
least 1.5 kg/cm2 over the acid pressures, to avoid the risk of plugging of ammonia
inlet to the reaction chamber.
If the acid pressure tends to increase steadily (the ammonia pressure will usually
increase as well) it could be indicative of a blockage. In any case, if it continues,
without having to shut down the plant or stop the other flows to the different
equipment, a P.R. steam flush will be done actioning HS-319/320, depending on the
PR. This will simultaneously stop the ammonia and acid flows to the PR to be
cleaned, which will be automatically re-established on switching the same HS-
319/320 off and stopping the steam flush.
Periodically, PR distribution tube shall be mechanically cleaned, if necessary, to

remove dirtiness coming from phosacid. This will be done from outside,
disassembling PR head last portion and cleaning pipe end portion with a screw type
tool similar to those employed for boiler pipes cleaning.
In all cases of DAP/NP/NPK production the PR temperature in TI-366/367 will be

between 125-145 C. If it is under 110 C it will be indicative of too diluted phosacid
feed and/or not enough ammonia feed. In the opposite situation the temperature
would increase over 150-155 C.
It's important to have a good molar ratio N/P control of the scrubbing liquid, as well
as of the scrubbing liquids solids content, which should not increase solids content
in the PR feeding liquor beyond 10%.
The slurries distribution inside the granulator (coming from preneutralizer and/or
pipe reactors) and the ammonization spargers performance will be observed. In the
granulator each one of the ploughshares has a blocking valve in case it is interesting
not to feed ammonia through one.
Obviously, it will also be checked that the product going to stores complies with the
specifications indicated in 6.2.
With the plant stabilized the systematic sampling and analysis as well as the control
of the parameters will begin as explained in Chapter 4.
Table 6.5.2 shows normal flows for each stream and main products, at 100% and
70% of nominal capacity.
TABLE 6.5.2
DAP 15-15-15
70% 100% 70% 100%
Ammonia
To 12-R-301A/B FE-333/334 4,9 7 1,7 2,45
To 12-R-302 FE-335 3,6 5,2 3 4,35
To 02-R-303 FE-342 - - 6,7 9,6
Phosphoric acid (48%)
To 02-R-303 FE-341 - - - -
To 12-D-311A/B FE-348 16,7 23,9 3,2 4,6
To 12-TK-301 FE-337 4,5 6,3 3,1 4,45
To 02-TK-302 Existing 2,3 3,3 1,54 2,2
To 02-TK-310 Existing - - - -
Sulphuric acid (98%)
To 02-R-303 FE-343 - - 4,9 6,95
To 02-M-361 FE-336 - - 0,49 0,7
To 12-D-311A/B FE-347 - - 1,7 2,45
To 02-TK-302 FE-351 - - - -
To 12-D-312 ACV-301 0.06 0.09 0,06 0,086
Water
To 12-D-312 Existing 7 10,3 14 20,1
To 12-D-311A/B FI-307 - - - -
Solids
12-WQ-327 WIQ-312 191 273 175 250
12-WQ-326 WIQ-314 40.6 58 44 63
02-M-401 WIQ-313 40 57 42 60
Transfers
To 02-TK-310 FE-344 7.7 11 15 21,7
To 02-TK-302 Existing 6 8,6 13,6 19,4
To 12-D-311A/B FE-346 7.7 11 13,5 19,3
To 02-R-303 FE-345 - - 16 22,9
To 12-TK-301 FE-332 25 36 0,7 1
To-12-R-301A/B FE-338/339 14,8 21,2 3,8 5,4
Slurry
From 02-R-303 FE-302/312 - - 17 24,55
From12-R-301A/B 21 30 5,6 7,9
6.6 NORMAL PLANT OPERAT ION. POTENTIAL OPERATIVE PROBLEMS
This section covers the description of the normal controls more specific of DAP and
15-15-15 manufacture, as well as the indication of the more common problems that
may arise and the way to prevent or solve them. All this assuming that the operators
have the knowledge and/or practice to be able to detect the problems and follow the
instructions indicated for the control of the different parameters.
The previous 6.5 Section dealt with the plant start-up operations, from the plant
preparation to its stabilization at its nominal capacity.
For its part, the following 6.7 Section will cover the plant shut down operations
including both normal and emergency shut down.
This Section assumes that the plant is in operation and stabilized, after the start-up,
to its nominal capacity, producing through mixed PN & PR process or single PR
process, depending on the manufactured grade:
Mixed PN & PR process: DAP, NP NPK SAB like 15-15-15
Single PR process: DAP
6.6.1 Normal plant operation. Parameters control
The plant is provided with control room computer screens, connected to a DCS
control system, and a general panel which includes the signalization of the main
working parameters for the different equipment and instruments in the plant. It also
includes a series of complementary elements such as motor amperimeters, alarms,
actioning buttons, etc.
Other parameters like FIs, PIs, etc. (See P&ID's) only have local signalization at the
site of the corresponding equipment.
With all this signalization and the different sample analysis that are systematically
performed, it will be possible to form judgement on the plant performance and
whether any operative parameter adjustment or equipment revision, etc., is required.
Most of the general controls to perform on the different equipment or plant sections
have been already described in Section 2.2. They will be complemented by the
specific controls for granulated DAP/NPK manufacture described next 6.6.1.1.
6.6.1.1 Process flows for liquid section and scrubber control for DAP and NPK.
Liquid raw material flows (phosphoric acid, sulphuric acid and ammonia) will be fed
as explained in Ch. 6.5.1.1, 6.5.1.4 and 6.5.2.
The distribution of the different liquid transfers between scrubbers is:
- Process water make-up is fed to 12-D-312 in all cases
- In 12-D-312 this water is mixed with a small quantity of sulphuric acid.
- From 12-D-312 the water is recovered into the Dust Scrubber seal tank 02-TK-
310, where it will be mixed with phosphoric acid, constituting the scrubber
liquor, in all cases.
- From 02-TK-310 is send to 02-TK-302 where is mixed with sulphuric acid and
more phosphoric acid where once more constitute the scrubber liquor.
- Liquor from 02-TK-302 is advanced to granulator pre-scrubber 12-D-311A/B,

where it is mixed with fresh phosphoric and with sulphuric acid.
- Liquor from 12-D-311A/B goes to PR feed vessel 12-TK-301 where it is mixed

with fresh phosphoric acid , in case of DAP production. Making 15-15-15, this
liquor flow from 12-D-311A/B is splitted between PR feed vessel 12-TK-301 and
Preneutralizer 02-R-303, under appropriate proportions.
- Liquor from 12-TK-301 goes to Pipe Reactor 12-R-301A or B or both.
Liquid transfer flows have been described in table 6.5.2
For the transfer flows between vessels the following rules will be considered:
- The quantity of water transferred between vessels will depend on the necessary
water to get a good liquid phase in the granulator. If the granulator needs only a
few quantity of water, the liquor flow to pipe reactor and the liquor transfer to
preneutralizer must be reduced. The transfer flow between vessels will
automatically decrease, and the densities in 02-TK-310/302 and 12-D-311A/B
will increase proportionally. Increasing these mentioned flows when the
necessities of water in the granulator are higher will get the opposite effect.
- Since normally all process water is introduced through the scrubbing system, if
water requirement is increased, the washing acid will become more diluted, with
advantages more evaporation, lower temperature and reduced risk of
crystallization for the ammonium salts formed.
The following parameters are expected in the scrubbing section:
Temperature washing liquid in scrubber vessels 02-TK-302/310: 55-65 / 30-40C
Average analysis of washing liquid in 02-TK-302/310 (depending on the grade):
%N = 2.4 4 / 0.5 -1,05
% P2O5 = 9 23 / 2-8
free% H2O = 60-80 / 85- 95
Rel. N/P = 0.77-0.9 / 0.64-0.65
At this conditions the crystallization temperature of the ammonium phosphate are

between 10-20 C, which means practically no cristallization problems in the second
scrubbing step.
Temperature washing liquid in granulator pre-scrubber 12-D-311A/B: 80-95C
Average analysis of washing liquid in 12-D-311A/B (depending on the grade):
%N = 4-7
% P2O5 = 40 45 for DAP

15 - 20 for 15-15-15
free% H2O = 25 30 for DAP

40 50 for 15-15-15
Rel. N/P = 0.4 - 0.5
At these conditions, the crystallization temperatures of the ammonium phosphate

are between 15C and 50C (at worst conditions, making DAP and NPK products).
Due to this, there is practically no problems in the scrubbing system in case of SAB
NP/NPKs production, but in case of DAP or other NPK production the washing acid
in 12-D-311A/B must be slightly diluted if the plant stops for more than 2-3 hours.
Nevertheless no problems are expected during normal operation since liquid
temperature will be always higher than 70 C.
However, is advisable to carry out the parameter control as has been described in
section 4.1 in order to detect the tendency of the values and take actions if needed.
For example, if the percentage of N in the liquid of the scrubber vessel 12-D-311A/B
is going up, without any appreciable change in the liquid density, it means that the
ammonia losses from the reaction are increasing due to some reason. In this case,
before the problem is identified and solved, could be interesting to change the
washing liquid composition to avoid the danger of crystallization (for instance, to add
temporarily more water or more phosacid, or more sulphuric acid).
6.6.1.2 Process flows for solid section.
Solid raw material depending on the formula (potash, filler) will be fed through their
correspondent feeder-weigher.
6.6.1.3 General considerations upon the common operative variables relatives to

the scrubbing liquids
a) Solubility
The different acid concentration indicated for scrubbing liquids correspond to high
solubility points of the salts formed in the reaction between the ammonia and the
phosphoric or sulphuric acids. The aim is to introduce in the system the minimum
amount of water, of course compatible with the functioning of tail gas and other
scrubbers, in order to reduce the amount of recycle needed inside the granulator,
obtaining the plant maximum production.
In chapter 7 there is a typical curve of the ammonium phosphate and ammonium

sulphate salts solubility in function of the ammonia and acid concentration.
Since this solubility is referred to the water content, it is obvious that for a higher
dilution of the scrubbing liquids there will be more dissolved solids and less risk of
blockages, although at the expense of an undesired increment of the liquid phase in
the solids bed, which will require a higher recycle, decreasing the production rate.
Similarly, if the ammonia looses to the scrubbers increase, high N/P values will be
obtained, the formed salts solubility will decrease and the scrubber liquids solid
content will increase.
During the plant operation, all efforts will be directed towards the minimization of the
NH3 looses to the scrubbers, all from the Preneutralizer 02-R-303, the Pipe Reactor
12-R-301A/B, and the granulator solids bed, and in a lesser extension the dryer. It
will be also tried that the cyclones work with the adequate removal efficiency, to
avoid too much dust going to the scrubbing section.
b) NH3 vapour pressure
NH3 pressure from the scrubbing liquid or slurry increases proportionally with the
molar ratio N/P for a given temperature. For instance, at molar ratio N/P = 1.0
(corresponding to a monoammonium phosphate MAP) and at 120 C ammonia has
a low vapour pressure, of about 2 mmHg; at N/P = 1.4 the pressure has reached 40
mmHg and, at N/P = 1.6 it exceeds 100 mmHg. The temperature also has some
effect on vapour pressure at a given N/P.
c) pH
For every different kind of phosphoric acid to be used in the new plant, it is
recommended to prepare titration curves, similar to the one enclosed in chapter 7,
neutralizing the phosphoric acid with same sulphuric acid content, at approximately
the concentration at which is going to be used in the scrubbing system, preferably
with ammonia. The curve must be representative of the scrubbing liquids with N/P
between 0.1 and 1.0.
With this experimental curves, just by measuring the scrubbing liquids pH, when
phosacid or phosacid plus some sulphuric acid is used, it will possible to quickly and
rather accurately estimate the corresponding N/P value, which will inform on the
plant operation. The N/P will, however, be confirmed with subsequent analysis.
In general, the scrubbing vessel liquids will operate at pH between 1 and 2,5.
6.6.1.4 Reaction section
The liquids feeding to the preneutralizer 02-R-303, that is Phosphoric liquor from
pre- scrubber vessel 12-D-311A/B, sulphuric acid and ammonia, will be controlled by
FIC from DCS. The same applies to the slurry tranferred from it to the granulator.
The molar ratio N/P analysis of the different sample of slurry leaving the PN will
inform us on whether the ammonia flow fed should be adjusted in order to take N/P
ratio to the desired value:
For DAP slurry : 1.45 - 1.5
For 15-15-15 slurry : 0.8 - 0.9
On the other hand, the temperature readings in TI-369/370 indicate if the reaction is
adequately developing. This temperature for DAP will usually be between 110-
120C, although fluctuations between 105-125C are acceptable. For 15-15-15,
where a lot of sulphuric acid is fed to the preneutralizer, slurry temperature is usually
about 10C higher, including fluctuation range. In all cases, if the temperature tends
to drop it could be due to a inefficient reaction, lack of ammonia or excessive dilution
of the incoming liquids. If, on the contrary, the temperature tends to increase, it
could be a sign of too concentrated liquids or too much sulphuric acid and/or
ammonia fed to the preneutralizer. This latter will be confirmed by an increase of the
ammonia losses to the scrubbing system, and an increase in the N/P and
temperature of its liquids.
The liquid level inside PN, LI-302/LI-303, will be closely observed during the
operation, trying to keep it between 60% of the total reactor height. If the level is too
low, there could be too many ammonia losses and affect the agitator performance. If
the level is too high, there is a risk of overflowing due to sudden foaming, etc.,
without giving the operators time to prevent it. The level, therefore, will be tried to be
kept as constant as possible by adjusting the flows fed to the preneutralizer and/or
the flow of slurry transferred from it to the granulator.
Defoamer has to be fed in continuos way, using defoamer-dosing pump, to avoid

problems of foam, which can produce slurry overflowing. It has to be tried to
minimize the defoamer fed flow due to economical reasons; this flow will mainly
depend on the acid impurities and it will be experimentally defined in each case.
The bottom of the preneutralizer will be checked for cold areas where there is no
reaction. This is due to local liquid ammonia flashes that produce some cooling,
making the product crystalize and even producing solidifications inside PN.
For its part, the Pipe Reactors 12-R-301A/B, are fed with liquid ammonia coming
from the main ammonia line, and phosphoric acid liquor coming from the 12-TK-301
vessel. Both flows are controlled by FIC from DCS.
Both in sections 2.2.3.2 and 6.5.2 a series of parameters, controls and operating
conditions for the PR operation have been explained.
Normal molar ratio N/P in the PR slurry is always between 1.35-1.5, not depending
on the produced grade (DAP, NP or NPK), in spite of that some times could be more
interesting to work at lower N/P ratio (1.0-1.3) if needed. When N/P exceed 1.5 the
ammonia loses from PR to the scrubbing system could increase and produce an
excessive N/P ratio and temperature in the scrubbing liquids, mainly in 12-D-
311A/B.
Sampling the slurry coming out of the PR distributor pipe is very difficult, as this
latter is located inside the granulator. It can be done with a device of the spoon
type, prepared for this purpose that can be introduced through one of the inspection
windows on the solids inlet side. This, however, is rather cumbersome and for the
PR control is usually enough with the reading of the FICs in the phosphoric and
ammonia inlet, as well as with the PR temperature and the analysis of the
phosphoric liquor fed from 12-TK-301.The temperature in TI-366/TI-367 should be
between 135-145C in normal operation. If the acid was more diluted than expected
and/or the ammonia feeding was smaller than required, the temperature would be
lower and the slurry would go to the granulator with higher humidity than necessary.
The opposite effect will appear if phosphoric liquor is too concentrated and/or too
much ammonia is fed to PR; in this last case granulation will tend to produce
excessive fine product.
Besides the permanent temperature indicators to panel / DCS TI-366 and TI-367, is
advisable to have in the plant a complementary temperature indicator, portable and
preferably of the digital type, to check the former reading and also to be able to read
the temperature in other points of the PR reaction heat and distribution pipe.
Making DAP or NP 15-15-15, under normal operation conditions, only one of the two
installed PR, either A or B, will be in operation. During the start-up, when DAP
was produced, both will be alternatively tried, observing simultaneously the physical
aspect of the slurries from the Preneutralizer with both PR, checking the distribution
over the solids bed in order that it is adequate.
6.6.1.5 Granulation loop equipment
As already mentioned, in section 2.2 have been described most of the general
controls to be monitored during the plant operation. The following points will also be
kept in mind, besides the ones indicated in Section 2.2 & 6.5.2:
a) Granulation
For DAP and for high ammonium phosphate/sulphate slurry containing grades, like
15-15-15 the moisture at the granulator exit should tried to be kept around 2.0%
because of its temperature tends to be high (around 95-100C) due to the slurry
latent heat and also granulator reaction heat. In this range of temperatures the salts
solubility is high and small increments in the solids moisture can increase too much
the liquid phase in the granulator solids bed.
For NPK grades, with less proportion of slurry content, the moisture at the granulator
exit used to be a little higher, around 2.5% in most cases. At the same time, the
granulation temperature will be normally lower, in the range 85-95 C depending on
the slurry proportion and the recycle ratio.
In both cases, this kind of products have a high solubility, as mentioned before, and
for this reason, the granulation conditions (H2O and temperature) are more strict
than for other products without or with less slurries content. In case of NP or NPK
products containing urea, besides that slurry, granulation moisture control is still
more strict and difficulties increases proportionally with its urea content.
If too much water is recovered into the process from tail gas scrubber or too much
diluted phosacid is fed to the system instead concentrated phosacid, the slurries will
be too diluted and the granulator's discharge too humid, tending to increase the
percentage of over-sizes. This will result in a frailer product, which will affect the rest
of the plant equipment, for instance, increasing the dryer fuel consumption, forcing
the crusher operation, impairing the screening, etc. Obviously, that effect will be
proportional to the amount of slurry in the formula, being more serious when
producing DAP or 15-15-15 and less serious in case of other NPKs
A side problem is that the granulator internals will be excessively wet, enhancing the
product sticking and accumulating on them, interfering with the operation and
decreasing the granulation yield.
If the solids bed temperature increased excessively, the raw materials solubility will
increase, tending to form more over-size product and favouring lumps formation
inside the granulator. Additionally, the ammonia looses to the gas granulatorpre-
scrubber 12-D-311A/B and also to the granulator scrubber 02-D-301A/B will
increase, increasing the scrubbing liquids N/P and making more easy to have
crystallization problems in the scrubbing system.
Product samples at the granulator exit will be periodically taken, according to what
was indicated in Section 4.1, which, besides for laboratory analysis, will be used for
the temperature, size and pH measurement in the plant itself.
The granulator operator will observe, a few times per hour, the granulation
performance, particularly in reference to the solids bed aspect and the product exit
moisture and granulometry. Also dust or ammonia emissions, gas suction, slurries
distribution, lumps formation or product accumulation on the internals, rubber panel
flexion, etc. will be checked. The observation of the slurry leaving the preneutralizer
and/or pipe reactor will be easier through the inspection doors on the inlet product
side. Through them can be also checked whether there is any problem of product
accumulation in the discharging area of the recycle product feeding chute, or even
over the main beam. One or more 150-watt lamps will be available at each side of
the drum, for its better inspection, in order to do these checks. With these
observations an experimented operator will be able to do any required plant
adjustment to keep the operation at its best.
During the time elapsed between two observations the inspection windows will be
preferably kept closed, especially the ones on the product discharge side.
Otherwise, the fan will suck a great deal of air from outside the drum, when it should
be sucked from inside, to remove the maximum steam and ammonia coming from
the solids bed and pipe reactor, as well as the dust generated from the solids bed.
The inspection window on the product inlet side will be partially opened in order to
favour the pass of air through the drum, which is what it is really needed for the
proper sweeping of its interior.
As already explained, the granulator has a grizzly, continuous with the drum, located
at the product outlet, which on turning enhances the breaking up of possible lumps
leaving the granulator. Nevertheless, if any of the lumps passed over it, falling out of
the dryer feeding chute, they would be immediately crushed with manual or
pneumatic mechanic hammers, re-feeding them to the dryer.
If any of the ammonia ploughshares in the granulator becomes blocked, the

ammonia injection to the solids bed would be momentarily stopped and steam
passed for about 1 minute, until unblocking it (do not forget to pass plant air after
steam). If after this time it was not unblocked and the feeding through that
ploughshare was considered essential for the correct operation, then the operation
will be stopped. An operator will be allowed to go inside, after taking all safety
measures required, to manually clean it. The operator will also check that the pipe
reactor distributing tubes slots and the preneutralizer distributing tube sprays are not
blocked, cleaning them if required.
The eventual slurry blockage at the pipe reactor outlet slots will be prevented as
explained during the plant start-up sequence, in section 6.5.2 and in the PR
description in section 2.2, passing MP steam through the actioning of the HS-
319/320 switch. The granulator operator, after gained some experience will be able
to detect any anomaly in the P.R., by the noise made by the slurry on leaving it.
Also the eventual slurry blockage at the preneutralizer distribution tube sprays will
be prevented by passing, manually, LP steam through the steam line 80-S1-A1-a-
111-H, stopping or not the slurry transfer, depending on the seriousness of the
detected initial blockage.
The granulator gases suction will be regulated, opening more or less the inspection
doors and adjusting the damper opening, to equilibrate the suction system and to
avoid nocive vapours and dust release within production building.
During the operation the ploughshares injection system performance will be

observed. The presence of lumps in the ammonia injectors supporting ploughshares
will be also checked in order to clean them during the next shut down. If they
impaired the granulation yield considerably, the plant should be shut down for their
immediate cleaning.
b) Drying
The dryer will remove any moisture excess of the product at the granulator exit to
values under 1.5% for all DAP/NP/NPK manufactured. Samples of product leaving
the dryer will be periodically taken, according to the sampling program, which will
serve as guide for the adjustment of the dryer conditions.
The natural gas feeding to the combustion chamber will be controlled depending on
the product, through the temperature of the gases entering or leaving the dryer.
The temperature of the dryer inlet gases should not exceed 200 C, being usual to
work around 150 C in order to avoid over solubility of the product entering the
dryer.
The temperature of the dryer outlet gases, when granulation temperatures are over
100-105 C is usually about 3-5 C hotter or cooler than the product leaving the
dryer. In extreme cases this temperature difference can be up to 8-10 C if the
product leaves the granulator with excessive moisture or too hot. The product
temperature at the dryer exit will be manually checked and should not exceed 100-
105 C, in order to avoid the product loosing too much ammonia (high N/P product),
which could prevent reaching the desired product grade. Also, it could increase the
N/P of the dryer scrubbing liquids as well as, later, that of the granulator with the
subsequent, already mentioned, problems.
If the product moisture is too high, it will be checked that the operation parameters
are adequate, as well as that the acid fed to the scrubbing system and/or pipe
reactor vessel is not too diluted, which is usually the cause of the problem.
Every time a sample is taken from the dryer exit, it will be checked the correct
feeding of the over size product not passing through the grizzly bars to the lumps
crusher. The amperage reading of this crusher will inform on its performance and on
any overloading.
For an experienced operator, the dryer electrical consumption evolution will be

indicative of an increase or decrease on dryer filling hold-up and. The plant load can
be directly observed from WIQ-312 in DCS. Both indications will also inform on the
product state, since for a constant recycle, the dryer filling hold-up should be
constant. If it increase it will mean a change in the product granulometry and/or
humidity, as the humid product tends to increase the hold-up.
In parallel with the reading of the exit dryer throughput in WIQ-312, the amperage
reading of the recycle elevator 02-M-305, will also inform on the recycled product
load.
c) Screening and over sizes crushing
The product leaving the dryer is transported and taken up to the product screening
and grinding section which is composed of four independent lines A, B, C, D. The
drag feed conveyors 02-DR-101/102 will distribute the product uniform all along the
product screens 02-F-301A/B/C/D. Resulting separated oversizes will be crushed in
the 02-Q-301A/B/C/D oversize mills.
If the oversize product cloth becomes blocked, the pulverizer will tend to be
overloaded, reducing its efficiency and favouring product accumulation in its walls,
due to the product entering with a very variable granulometry and some dust. In this
case the pulverizer amperage reading will increase significantly. On the other hand,
it will make too much on-size product go to the recycle decreasing the unit
production and reducing the crushing efficiency, being the recycle over sized,
producing granulation problems.
If the product reaching the screens and pulverizer is too wet, it will be frailer and
break more easily producing excessive dust that will go to the scrubbers, causing
the already mentioned problems on scrubbing liquids.
If the pulverizer amperage reading increases without any sign of a higher

percentage of oversizes at the granulator exit neither the screen cloth being dirty, it
could be indicative of product accumulation in the pulverizer walls or mobile parts,
being recommended to clean it during the first shut-down you have to do, or even do
an emergency shut-down if the amperage increase is very high.
If the fine clothes of the fines screens in 02-F-301A/B/C/D were dirty, the fines will
pass to the unit exit, overloading the rotary cooler 02-M-363 and the polishing
screen 12-F-302 and favouring the presence of fines in the commercial product and
increasing its temperature. The fines screen clothes should, therefore, be clean,
being periodically examined by the corresponding operator.
d) Transport equipment and recycle regulation
The transport equipment is provided with motor shut down mechanisms in case of
serious blockage. Also, due to the plant interlocking system (See Section 2.3), this
shut down may cause the immediately previous equipment shut down.
Again, the amperage consumption will be indicative of its performance and of any
anomaly.
By changing the speed of the product feeder conveyor 02-D-326 the product
recycled to the granulator will change accordingly. Depending on the granulator
operative conditions, it may be necessary to increase or reduce the recycle,
respectively reducing or increasing the belt conveyor speed, in order to extract less
or more product than the corresponding to the total plant raw materials feed. In this
case, the product load in the granulator loop will change at a t/h rate equal to the
hourly tonnage difference (dry base) between the plant extracted product and the
raw materials fed. For instance, if the plant is stabilized with a feeding of raw
materials for 50 t/h production, but the system seems capable of working at a lower
recycle ratio, the commercial product extraction could for instance be increased to
55-60 t/h, the instant product load inside the granulation loop being decreased at a
rate of 5-10 t/h. After some time and with the plant working in the adequate recycle
conditions, the product extraction will be re-established to be in accordance to the
raw materials feeding rate.
6.6.1.6 Dedusting and gas scrubbing
The plant is provided with a series of cyclone batteries to catch and remove the dust
carried by the air entering the cyclones. Before and after the cyclones there are
points for measuring the system's pressure, which will inform on the pressure drop
through them. This pressure drop should be between 80 and 150 mm w.c. Any
reading outside this limit will be normally indicative of a system malfunction. If the
cyclones' entrance becomes blocked the pressure drop will increase and the gas
flow will be reduced. This may cause not enough dust being removed from the
equipment producing and excessive dust emission inside the plant, near the
equipment, with the subsequent inhabitation problems of the area. On the other
hand, if the product is not conveniently unloaded from the cyclones, and they loose
the "cyclone" effect, the separation efficiency will decrease and the excessive dust
going to the scrubbing causing the problems mentioned in Section 6.6.1.3.
It is advisable to periodically check all pressure drops in all the plant cyclone
batteries.
The scrubbing towers have PDI installed between the scrubber gases inlet and
outlet, whose readings should always correspond to the values indicated by the
suppliers. The reading values will depend on the flow regulation to the tower and
venturi and therefore it will be checked that they are correct. Deviations from the
indicated pressure drops will be indicative of lack of liquid or air, if they are lower, or
product accumulation, if higher.
Each scrubbing liquid spray must have its own valve, in case one of them should be
isolated.
If in any of the lines to the sprays, with the valve open, is detected a temperature
lower to the others, it will be indicative of a possible blockage, which should be
cleaned during the next scheduled shut down.
6.6.1.7 Commercial product treatment until plant outlet
The commercial product extracted from the granulation loop by the product feed
conveyor 02-D-326 is sent to the Rotary Cooler 02-M-363 to bring its temperature
down.
The DAP/NP temperature at the cooler exit will be 50-55 C maximum, and the NPK
temperature will be 60C maximum.
When chilled air is used, it must be desaturated in 12-E-304 by setting the desired
temperature in TIC-355 from DCS. An increment of 4-6 C in the air temperature
should be enough to decrease its relative humidity up to 70-75%. Any way, it must
be adjusted from psycrometric graphics and air temperature in the exit of 12-E-302
(TI-357). Higher increase (about 10C) may be requised when producing urea based
NPKs, to decrease relative humidity to 58%.
After cooling, the product is screened in polishing screen 12-F-302, in order to

remove the possible remaining fines and oversizes from the commercial product.
Periodically it will be examined that the cloths are clean, so that the fines are not
dispatched with the final product to stores or too much product is recycled.
The amount of product leaving the plant will be indicated and totalized by the WICQ-
313, installed on the product belt conveyor 02-M-401 going to stores. Previously the
sampler 12-SP-401, located in the chute between the polishing screen and the final
product belt conveyor, will take samples of product for its analysis.
6.6.1.8 Other equipment
a) Defoamer
If when observing the liquids of the different vessels 12-TK-301, 02-TK-302/310 and
12-D-311A/B some foam tends to be produced, which is normal when phosphoric
acid is used as a washing liquid, it may be necessary the addition of some defoamer
through the pump 12-P-316. Foam can also be present in the preneutralizer 02-R-
303 due to strong reaction in it.
It will be important to add the minimum amount of defoamer, strictly the necessary
one, in order to not to increase the product cost and because too much defoamer
sometimes can, paradoxically, produce more foam. In general, we will start by
working at 10% of the dosing pump scale, gradually increasing this amount, if
needed, until there is no more foam observed. Periodically (at least once every two
hours) the pump will be stopped to see if the cause producing the foaming remains
or not.
b) Solid raw materials feeding
Solid raw materials, potash ammonium sulphate TSP, urea and filler, will be fed in
parallel through their correspondent feeder/weighers WICQ-307/308/309/310/311.
The flows must be set from Control Room according to the grade to be
manufactured and after being checked the real composition of the raw materials to
be used.
It has been already mentioned that is very important not to make mistakes when
filling the bins in order to avoid serious deviations from the nominal grade
composition in the final product.
The bins have a high and low-level alarms, which will indicate when to stop or start
its filling.
The bins are also provided with a big blaster system to avoid arching when the
products have some tendency to cake; when this happens, the flow through the
weighers becomes zero, being detected by the alarm and, in this case, the operator
must switch the correspondent big blaster in order to reestablish the flow through
the weigher.
Do not forget that absence of flow through any weigher can cause deviations of
analysis in the final product if solid raw materials are used in the product
composition.
c) Utilities supply
For a correct plant operation the specifications and required utilities quantities
should be guaranteed (See Section 1.3.4): plant and instruments air, MP steam, LP
steam, process water and natural gas, etc.
6.6.1.9 Adjusting the product grade
It should be stressed that any change in the composition of the raw materials
feeding or, with a lesser importance, in the yield (NH3 and dust recovery) will
relatively affect the product nutrients content. If some adjustments are required,
they will be made with great precaution, making small changes and giving them time
to notice their effect, before more corrections are needed.
The following basis will be kept in mind:

1. The product is sold with a minimum guaranteed content of nutrients. Generally,
lack of nutrients will result in a penalty payment. On the contrary the client
welcomes nutrient excess, but represent an unnecessary additional cost to the
producer.
2. The filler and sulphuric acid addition reduces the percentage of all other
nutrients.
3. The addition of an excess of sulphuric acid allows to easily increase the N

percentage in the formulation, provided the corresponding NH3 is added to react
with it. However, it will also have a diluting effect on the other nutrients as it acts
as filler.
4. The impurities and sulphuric acid contained in the raw phosphoric acid fed to
the plant will have the same respective effect than indicated in previous
paragraphs.
5. An excess of any raw material can increase the correspondent nutrient analysis,
but it will decrease the percentage of the other nutrients. The opposite effect is
also possible.
6. If the nutrient percentage of the raw materials are not the expected, the
formulation must be re-calculated according the actual analysis and, the new
figures will be set on the flowmeters and weighers.
7. Big and frequently variations on the recycle ratio due to a bad granulation
process, can also produce important deviations in the final product analysis,
even if the raw materials flows are normal.
8. The water contained in the product acts as filler but, due to its small percentage,
its effect is minimal.
With this basis in mind the operator will adjust, at least every four hours, the raw
materials feed flow according to the laboratory results of the product analysis.
6.6.2 Operative problems analysis and correction
The following sections will examine the specific problems that may arise in the plant
and the recommended corrective measures.
The PN operation works around the following parameters:
1.1 Tendency to the PN slurry solidification. In these conditions the preneutralizer

slurry viscosity increases. It is generally detected by an increase in the slurry
transfer pump motor amperage readings as well those of the agitator.
Possible causes:
1.1.1 Dense scrubbing liquid / insufficient water.
1.1.2 Excessively low PN molar ratio N/P (little reaction ,low temperature, high
viscosity).
1.1.3 Excessively high molar ratio N/P (too much reaction, excessive
water vaporization , excessive slurry concentration).
1.1.4 High specific gravity.
1.1.5 Temperature too low.
1.1.6 Temperature too high.
Corrective measures
1.1.1 See section 6.6.2.3.1 of this Chapter.
1.1.2 Add ammonia until the molar ratio N/P is adequate.
1.1.3 Reduce ammonia feeding until the molar ratio N/P is adequate.
1.1.4 Check solids content and N/P in the scrubbing liquid from 12-D-311A/B
and its flow. See previous paragraph 1.1.3. Add water.
1.1.5 Check all feeding flows to PN. Open concentrated phosacid valve and
reduce transfer of phosphoric liquids from 12-D-311A/B. Increase
ammonia to PN.
See paragraph 1.1.2
Check molar ratio N/P. Check sulphuric acid flow and its density.
1.1.6 Mechanisms opposite to paragraph 1.1.5
See paragraph 1.1.3
NOTE : If the preneutralizer slurry becomes to thick to be pumped, stop the ammonia, phosphoric
acid, sulphuric acid and scrubbing liquid feeds completely and dilute the PN content with
water. If, besides, the temperature is too low, steam can be added. Meanwhile, reduce
production to stores proportionally. If the problem was such that it is not corrected in few
minutes, all the system will be stopped. It should be remembered that if, in an extreme
case the preneutralizer slurry became solid, its content should be manually removed with a
pneumatic hammer. In these conditions special care should be taken when trying to break
the superficial hard crust as the hot slurry inside might cause serious burns.
2.1 PG-328/329 pressure (liquid ammonia line).
2.1.1 PG-328/329 pressure increase (liquid ammonia line)
Possible causes:
2.1.1.1 Increase in the ammonia supply pressure at B.L.
2.1.1.2 Blockage in PR distribution pipe or ammonia inlet to reaction head.
2.1.1.3 Flows increase.
Corrective measures
2.1.1.1 Regulate ammonia pressure at B.L.
2.1.1.2 Flush PR with steam. Check NH3 and acids feed flows as well as the
pressure in all PR lines. Remember that NH3 pressure should be at least
1 kg/cm2 higher than the phosphoric acid pressure.
2.1.1.3 Re-establish flows or open more the slots free exit area in the PR
distribution pipe.
2.1.2 PI-103 A/B pressure decrease (liquid ammonia line)
Possible causes
2.1.2.1 Decrease in the ammonia B.L. pressure.
2.1.2.2 Liquid ammonia feeding conditions problem (pump).
2.1.2.3 NH3 flow significant decrease.
Corrective measures
2.1.2.1 Check liquid ammonia conditions at B.L.
2.1.2.2 Check supply from storage. If needed use another pump normally
installed in parallel.
2.1.2.3 Check and re-establish NH 3 flow.
2.2 PI-331/332 pressure (phosphoric liquor line)
2.2.1 PI-331/332 pressure increase (phosphoric liquor line)
Possible causes
2.2.1.1 Increase in feed flows to PR.
2.2.1.2 Blockage in PR distribution pipe or in phosphoric liquor inlet to reaction
head.
Corrective measures
2.2.1.1 Adjust flows. If the pressure is too high from the beginning of the
operations, open more the slots free exit area in the PR distribution pipe.
2.2.1.2 Do a steam flush.
2.2.2 PI-331/332 pressure decrease (phosphoric liquor line)
Possible causes
2.2.2.1 Decrease in feed flows to PR.
2.2.2.2 Phosphoric acid pump 12-P-315A/B/C malfunction.
2.2.2.3 Blockage in phosphoric line from 12-TK-301.
Corrective measures
2.2.2.1 Adjust flows.
2.2.2.2 Check pump. If needed use the pump installed in parallel.
2.2.2.3 Check line blockage. Flush line with water and/or steam. Check N/P in 12-
TK-301 liquid.
2.3 P.R. temperature (TI-366 / TI-367)
2.3.1 TI-366 / TI-367 excessive temperature
Possible causes
2.3.1.1 Main cause: Excessive NH3 in PR.
2.3.1.2 Significant increase in the concentration and/or temperature of the
phosphoric liquor fed from 12-TK-301
Corrective measures
2.3.1.1 Check NH3 flow and N/P.
2.3.1.2 Adjust acid concentration and phosacid feedings (weak-strong) and check
temperature of the transfer liquids from 12-D-311A/B to 12-TK-301.
2.3.2 TI-366 / TI-367 lack of temperature
Possible causes
2.3.2.1 Lack of NH3 in PR.
2.3.2.2 Defective mixing in PR. Little pressure in distribution tube.
2.3.2.3 Significant increase in the phosacid acid dilution.
2.3.2.4 TI-366 / TI-367 defective reading.
Corrective measures
2.3.2.1 Check NH3 flow.
2.3.2.2 Partially close the slots free exit area in the PR distribution pipe, by
moving the collar or bracelet. Change the ammonia injection nozzle.
2.3.2.3 Check concentration of the acids fed. If needed increase it or decrease

the amount of water from scrubbing section. If feasible add temporarily
more concentrated phosacid directly to 12-TK-301.
2.3.2.4 Check TI-366 / TI-367 temperature with a digital portable thermometer.
Repair or reset sensitive element in TI-366/367.
6.6.2.3 Scrubbing liquids
3.1 Liquid too dense or thick

It is generally detected by an increase in the motor amperage readings of the

scrubbing liquid circuit pumps, vessel transfer pumps, and agitators of the scrubbing
vessels 02-TK-302/310 12-D-311A/B or PR vessel 12-TK-301.
Possible causes
3.1.1 Excessive dust carried: cyclones malfunction or excessive dust emission
in the units.
3.1.2 pH too high. Molar ratio N/P too high.
3.1.3 Too high concentration.
Corrective measures
3.1.1 Check cyclones dust discharge and, if needed, clean discharge valves.
Check equipment dust emission and granules fragility. Add water to
affected scrubbing unit.
3.1.2 Possible excessive NH3 looses: if from dryer to dryer scrubber due to
excessive temperature, reduce temperature if needed; if from
granulator/PR/PN to granulator pre-scrubber, check granulator solids bed
(quantity, granulometry, humidity) and act in consequence; check PR/PN
molar ratio N/P and solids pH at granulator outlet. Check NH3 flow to all
equipment, flows and concentration of acids to PN and/or PR.
3.1.3 Check phosacid feeding flows (weak and strong) to scrubbing system and
re-adjust its if necessary. Add water temporarily to affected scrubbing unit.
Check liquid transfer between vessels.
3.2 Scrubbing liquids % N too high
In DAP/NP/NPK manufacture % N values in 12-D-311A/B and 02-TK-301 should not

exceed the critical crystallization point according the dilution of the phosphoric acid
used (see solubility curves). Higher values will be indicative of scrubbing
malfunction. It should be remembered that at higher % N and temperature there will
be higher NH3 looses to the tail gas scrubber. Check correct phosphoric or sulphuric
acid feed to scrubbing system.
Possible causes
3.2.1 Excessive N/P in PN or PR.
3.2.2 PN slurry level too low.
3.2.3 Excessive temperature in PN, PR, granulator or dryer.
3.2.4 Deficient NH 3 distribution at granulator.
3.2.5 Deficient slurries distribution in granulator.
3.2.6 Excessively dry operation conditions which favour NH3 and dust loses.
Corrective measures
3.2.1 Adjust NH3 and/or phosacid or sulphuric acid flows to PN.
Adjust NH3 and/or phosacid acid flows to PR.
3.2.2 Check flow at PN inlet at outlet.
3.2.3 See paragraph 1.1.6 and 2.3.1.

Enhance pass of air through the granulator: close inspection doors on the
product exit side, open windows on inlet side. Reduce temperature of
drying air.
3.2.4 Steam-flush any blocked injector of PN or granulator ploughshare. Check
possible break in NH 3 feed pipe to injectors inside the granulator.
3.2.5 Check PN and/or PR slurry distribution inside granulator. Steam flush if
needed.
3.2.6 Check concentration in scrubbing system and PN slurry density. Dilute if
needed. Temporarily add water directly to granulator.
It should also be remembered that the higher scrubbing liquids N/P is, the higher the
NH3 looses will be. High scrubbing liquids N/P will be significative of high reaction in
the tower and, therefore, increase in the recirculation liquid temperature, favouring
even more the looses. In this case it will be convenient to dilute the liquids feed to
the scrubbing vessels, increasing the water/ acid proportion if needed.
6.6.2.4 Granulator
4.1 Product too wet at granulator outlet
Higher humidity than the necessary to have a good granulation yield will mean
higher oversizes percentage due to a liquid phase increase. This will increase the
recycle and reduce the production capacity. It will also mean higher fuel
consumption in the drying. If the product moisture is excessive (>2.5-3.0%
depending on the grade) it may become too brittle, easily breaking and producing
dust.
A product too wet can also favour lumps formation inside the granulator, blockage of
the chute from the granulator drum to the dryer, product accumulation on the dryer
flights, impairing the drying and favouring the exit from the dryer of big product
lumps not properly dried.
Possible causes
4.1.1 PN and/or PR slurries too diluted or in excessive amount.
4.1.2 Low granulator pH.
4.1.3 Low recycle ratio.
4.1.4 Too diluted acids entering the plant.
4.1.5 Uncontrolled, unforeseen water feeding to the plant.
4.1.6 Deficient granulator's air swept.
4.1.7 Too wet recycle.
4.1.8 Shut down of any solid raw materials feeder.
Corrective measures
4.1.1 Check PN and/or PR flows, ammonia and acids. Check concentrations
and molar ratios N/P in PN/PR. Increase phosphoric liquor concentration.
4.1.2 Check NH3 flow to granulator ploughshares and NH 3 looses from solids
bed (% N in scrubbing system). Correct ploughshares inefficiency, check
if there is any blocked.
4.1.3 Reduce product extraction from granulation loop to stores. Check that
recycle is not too over-sized: check pulverizer functioning.
4.1.4 Check respective acid flows and its densities (strong and weak phosacid
and sulphuric acid). Reduce water/acids ratio or adjust strong-weak
phosacid ratio if needed.
4.1.5 Check that all water inlet valves are closed.
4.1.6 Close inspection doors on granulator's product exit side, open windows on
inlet side. Slightly open air suction on granulator's product inlet side, if
needed.
4.1.7 Check recycle humidity, increase air flow to the dryer and its temperature,
if needed.
4.1.8 Check feedings of KCl , Filler or other raw material and eventually
recovered spillages and reestablish flows.
4.2 Excessive solids bed temperature
In DAP, NP or NPK manufacture with high amount of slurry content the temperature
at the granulator exit will usually be between 95-100C. Temperatures continuously
over 110C can favour a significant increase of the ammonia looses to scrubber,
increasing its scrubbing liquid % N, and a tendency to increase the oversizes
percentage in granulator, that will force the pulverizer operation generating more
dust to the scrubbers. In case of manufacturing products with high urea content, that
usually granulation temperatures are between 85-95 C, is not convenient, due to
the same related reason, to exceed 100 C.
Possible causes
4.2.1 Excessive temperature in PN and/or PR slurries.
4.2.2 Lack of recycle.
4.2.3 Lack of air through the granulator.
4.2.4 Recycle too hot.
Corrective measures
4.2.1 Check PN and/or PR slurry temperature. Adjust NH3 feed flows if
excessive. Dilute phosphoric liquor fed to PR. Check sulphuric acid flow to
PN , specially when making NP grades with high sulphuric acid content.
4.2.2 Reduce product extraction from granulation loop increasing the recycle.
4.2.3 Increase granulator suction. Close inspection doors on the product exit
side, open the ones on opposite side. Slightly increase air suction from
the product inlet side.
4.2.4 Check drying temperature.
6.6.2.5 Other general preventive measures
Paragraphs 4.1 and 4.2 lead to granulate oversizes. In case of fine granulation it
would be due to low temperature or lack of liquid phase which is composed of water
(humidity) and dissolved salts (depending on water and temperature). In these
cases the corrective measures would be opposite to 4.1 and 4.2.
The different equipment ammeter readings will indicate the corresponding

equipment load. Any abnormal fluctuation of those readings will generally be
indicative of an anomaly that will be examined and corrected.
The chute from the granulator to the dryer will be closely observed to avoid the
product pasting and blocking it. It will be tried to keep it clean at all times. (Cleaning
is usually performed with the plant in operation, with steel bars and even with
pressurized water).
The screens will be periodically examined, checking that the product is well
distributed all along the cloths and that these are clean, otherwise crusher will be
overloaded (sending on-size product back to the granulator) or too many fines will
be passing with the commercial product. Also, a hole in the oversize cloths may let
product over 4 mm go to polishing screen and then to stores.
A good crushing efficiency should be kept. The crusher operation will be indicative
of the granulation performance. Thus, if its load tends to increase it might be due to
the oversize granulation (and/or the oversize clothes of process screens being dirty)
or to the product arriving too wet, tending to paste and accumulate inside the
crusher.
Periodically, the inner chains will be checked and the corresponding cleaning done.
Product can accumulate both inside the fans casing as in their impeller flights,
unbalancing them and causing vibrations. During the plant shut- downs they will be
opened and cleaned.
Product will progressively accumulate in the suction and gas transport ducts. The
evolution of the pressure drops in these equipment will be indicative of their
condition and whether they should be cleaned. This will be done through the
inspection doors with metallic rods and even steam if needed.
Sometimes big product lumps can be formed in the granulator or dryer. If this
happens and they are not broken up during operation or by the grizzly bars installed
on those drums, it may be necessary to shut the plant down for a short period of
time in order to break them up or remove them from the system.
Finally, remark the importance of checking the pH at the granulator exit, which will
be indicative of any excess or lack of ammonia.
6.7 PLANT SHUT -DOWN PROCEDURE
With this type of plant it is customary to program the periodic plant shut-down in
order to proceed to the normal cleaning, repairs needed and equipment
maintenance. This shut-downs take place usually once a week or every two weeks,
although they may vary depending on the plant management philosophy production
requirements and on if there is an emergency repair or cleaning required. On
programming the plant shut-downs it should be kept in mind that an ordinary plant
shut-down, when rutinary equipment cleanings and checkings take place, will help
avoid future unprogrammed emergency shut-downs due to serious impairment of
the plant operation conditions or equipment break down.
There are two types of scheduled plant shut-downs depending on whether the shut-
down will be relatively short lasting, without emptying the granulation loop; or long
lasting, having to empty all the installation. For these two situations that from now
on will be called ordinary scheduled shut-down and long-term scheduled shut-down,
two different shut-down procedures will be followed. Besides, once a year, the plant
will be shut down for 1-2 weeks in order to proceed to thorough cleanings,
checkings, maintenance, equipment parts replacement, etc. This situation is referred
to as annual plant shut-down, which in fact is a particular case of the long-term
scheduled shut-down but more thorough and practically applying to all the
equipment.
Finally, as in all production plants, there can also be the plant emergency shut-down
enforced by the serious breakdown of essential equipment or serious impairment of
the plant operation conditions. These shut-downs can be either short or long lasting
depending on the cause.
6.7.1 Plant scheduled shut-downs
For the ordinary and long-term scheduled plant shut-downs two different procedures
will be followed. In the first one most of the plant will remain loaded and ready to go
on with the operation, while in the second one the plant will be emptied and re-
loaded before re-starting it.
6.7.1.1 Ordinary scheduled shut-down
In this shutdown the Preneutralizer will remain loaded, if employed, and the
scrubbing vessels will be emptied in order to wash them with water. The elevators,
screens, crushers, etc., will be also emptied storing their load in the granulator and
dryer.
The sequence of steps will be the following:
Previously to begin any shut down sequence, all liquid stored in the sump tank must
introduced to the scrubbing system. As this operation can take some hours is
advisable to foresee it with enough time.
When it is decided to shut down, the water feed to 12-D-312 will be stopped as well
as the sulphuric and phosphoric acids feeding to the scrubbers. Liquid will be kept
recirculating through the scrubbers, the transfer must be keeped as usual, at normal
rate, until the minimum level in vessels is reached. Then the corresponding valves
will be closed in order to stop the liquid transfer from scrubbing section to pipe
reactor vessel and preneutralizer.
It should be mentioned that during the minutes 12-D-312, 12-D-311A/B and 12-TK-
301 take to empty to their minimum level (required by the pump) the % N and dust in
the recirculation liquid will have significantly increased, due to the lack of fresh acid
and process water feed to the vessels and the reduction to minimum of the total
liquid in the system. It should, therefore, be checked that there are not blockages in
it. It will also be checked that the temperature does not increase excessively,
damaging the material the equipment is made of. If needed, controlled quantities of
water can be added to granulator pre-scrubber and scrubber seal tank. Operating
fan dampers will also control the gas flows to the scrubbers.
These preventive measures will also apply during the subsequent emptying of 12-
TK-301. During this period ammonia flows to P.R. and granulator can be reduced, in
order to minimize losses to granulator pre-scrubber 12-D-311A/B. When this vessel
is emptied until its minimum level, the ammonia and acid feed to the P.R. can be
stopped.
After being stopped all feeding flows to PN, slurry transfer from it to granulator can
also be stopped. At this moment, the LP steam to the PN will be opened in order to
keep it hot avoiding cristallizations. All ammonia valves to the PN will be closed.
Ammonia flow to granulator has to be proportionally reduced to avoid excessive

losses.
Now, the ammonia and acid feeds to PR can be stopped.

Once stopped PR flows, HS-319/320 will be switched on in order to flush PR with

steam. The ammonia valves to PR will be closed. The flush will last for about 2
minutes. More or less 30 seconds later, the ammonia feed to the granulator will be
also stopped as well as the ammonia pump. This little extra time that the ammonia is
allowed to flow to the granulator is to let the solids bed dry, preventing lumps or
pasted areas remaining in it.
In parallel solid raw material feeders, and any liquid flows to the granulator (water,
sulphuric acid, and steam) will be also stopped.
In order to not leave the plant too empty of product during the shutdown period, the
product feeder 02-M-401 will be stopped, keeping the product in a closed circuit.
Then 10-20 minutes later the burner will be stopped. For this purpose it will be
progressively taken to its minimum level and, from the dryer control panel, the fuel
oil and combustion air feed will be also stopped. The quench air will be left on. (For
more details about this operation see the "Operation Instructions" from the burner
vendor).
Next, the dryer will be stopped keeping the granulator in operation, as well as the
remaining granulation loop equipment. As each equipment becomes empty, they all
will be successively stopped, from the dryer lump crusher to the recycle elevator,
passing by the remaining intermediate granulation loop equipment such as
conveyors, screens, pulverizer, etc. At last the granulator will also be stopped, the
throughput remaining stored between the granulator and the dryer.
The equipment for the product extraction from the granulation loop, to stores will be
stopped, once all the system is empty of product.
While all that is being stopped, the scrubber fans will also be stopped, ceasing the
recirculation back to scrubbers and passing as much as possible of the nutrient-rich
remaining liquids to the PR vessel 12-TK-301 or to the preneutralizer 02-R-303 in
case of cleaning of 12-TK-301.
Next, water will be added to 12-D-311A/B, 02-TK-302/310 and 95-WC-05 until it

reaches 50% level. They will be then recirculated for over 2 hours to facilitate the
system's washing. The recirculation pumps are then stopped together with the
scrubber fans. Finally the liquid in scrubber tanks will be drained to the sump tank.
Normally, only PR vessel 12-TK-301 will remain full or partially full of liquid. If this
vessel cleaning is also foreseen, its liquid content must be transferred to 02-TK-302
or 310 after being both cleaned. This transfer can be done by means of a portable
pump and a suitable flexible hose.
During this ordinary scheduled plant shut-down the following cleanings and
checkings will take place:
a) Piping, pumps (lubrication...), tanks (and their agitators) and scrubbers

(including sprays).
b) Fans and ducts.
c) Inspection inside and product lumps removal from: granulator, dryer, cooler,
cyclones, crusher and chutes.
d) P.R., slurry distribution pipes and sprays, ammonisation ploughshares and

granulator lining.
e) Conveying equipment.
Particularly in the granulator, any pasted product in the supporting structure,

ammonia ploughshares and distribution pipes will be removed.
Once completed the washing and with the fans stopped, the scrubber manholes will
be opened in order to clean the scrubbers, re-starting the fans with their dampers
50% open. This will get rid of any generated vapours that might harm the operators
while inspecting and cleaning. The drop separators and packing will also be
inspected.
Once the scrubbers are clean, stop the fans in order to check and clean them.
When all repair, cleaning and maintenance operations are completed, the plant will
be re-started following what was explained in Section 6.5.1 for the scrubbers filling.
The recycle system will be started in a closed circuit, being the plant in condition to
be re-started according to what was detailed in Section 6.5.2. At this point should be
remembered that cleaning acidulated water from sump tank, which will be practically
full, must be re-introduced to the scrubbing system as soon as possible in order to
keep that tank almost empty, with enough capacity to prevent any leak from
scrubbing equipment when re-starting the unit.
6.7.1.2 Long-term scheduled shut-down
This is the procedure to follow when the plant is going to be shut down for a long
period of time or when it seems convenient to empty the plant completely, including
the preneutralizer and all the granulation loop. These shut-downs are usually
scheduled in order to perform the monthly maintenance operations or as
consequence of market conditions, production planning or a serious break down in
one of the essential equipment, leading to an emergency shut-down.
The shut-down procedure will be initiated similarly to the previous ordinary shut-
down (See 6.7.1.1), but trying to get the minimum slurry level in the preneutralizer
before stopping feeding and without stopping the granulation loop, neither the final
product section to storage.
The scrubber pumps will be re-started, washing only with water all the scrubbing
system and keeping all transfer lows closed and keeping the level in all scrubbing
vessels at about 50-60% with water. Also fans will be re-started.
In case of shut-down after being used a process with PN, the plant will be again
started in recirculation with the burner at its normal level and the slurry from the PN
will be transferred to the granulator until PN is practically empty. All solid and liquid
raw materials will remain stopped. During this time some liquid ammonia will be feed
to granulator to ensure the correct product pH. The slurry temperature inside the
preneutralizer has to be controlled and more steam fed if it tends to go below 100C.
The product extraction from product feeder conveyor will be increased as much as
possible, according the transport capacity from this point to storage, in order to
empty the granulation loop in a short time.
In case of NPK production, when PN is not used, during this last phase of plant
shut-down, the granulation should continue to reduce the recycle before emptying
the plant, using steam and/or water coming from 12-D-312.
When the quantity of product going to the storage is lower than 5-10 t/h, the product
leaving the elevator will be sent to the seed room.
The removed product throughput will be used to fill the plant for the next DAP, NP or
NPK manufacture.
Meanwhile, the product exit line: cooler, product elevator, polishing screen, etc., will
have been stopped.
Once all the recycle has been emptied, more water will be fed to the scrubbers,
keeping the recirculation to the scrubber towers for 2 hours in order to clean them.
Water will be also passed through the transfer lines between scrubber vessels.
Once the washing is completed, the pumps will be stopped and the vessels drained
to the sump tank. The vessels and scrubbers will be now opened for their inspection
and cleaning. In this case, if all vessels must remain empties for maintenance, the
acid content in PR vessel 12-TK-301 must be transferred to a provisional storage
instead 02-TK-302 or 310 as it is already told before.
Simultaneously with the granulation loop emptying, water will be added to the
Preneutralizer, filling it up to maximum level. The agitator, which was stopped when,
during the slurry emptying operation, the PN level was below the minimum required
(about 2 m from the bottom), will be re-started.
Steam will be fed to the PN through the ammonia injectors, keeping the PN in
agitation with hot water for two hours, after which time the two slurry pumps and the
corresponding transfer lines will be washed with that hot water at about 60C.
During the washing it will be necessary to keep on feeding water and steam, in order
to keep the system hot and the agitator sufficiently covered with water.
Once all the recycle has been emptied, more water will be fed to the scrubbers,
keeping the recirculation for two hours in order to clean them. Water will also passed
through the transfer lines between scrubber vessels and PN and also PR vessel if
emptyed for their cleaning. Once washing is completed, the pumps will be stopped
and the vessels and PN drained. All that vessels and PN will be now opened for
their inspection and cleaning if needed.
Once stopped the granulation loop, the interior of the granulator and dryer drums will
be inspected and, if there were a considerable amount of stuck product, these
equipment will be cleaned using pneumatic hammers. At the end of these cleanings
and during this long shut-down all the maintenance operations indicated for the
short shut-down (See 6.7.1.1) can be performed on top of the recommended
monthly revisions or any that the Maintenance Department might have programmed.
When all those operations have been completed and it is decided to re-start
production, it will be started by the preparation operations indicated in Section 2.5.1
for the vessels filling with the required liquids, the plant loading with product
extracted from a previous similar production, and plant start-up in the usual way.
The remaining operations are the same described in the previous section.
6.7.1.3 Annual plant shut-down
With this type of plant it is customary to program an annual shutdown for 1 or 2

weeks, to perform all maintenance operations of great magnitude and comply with
the revision programs foreseen by the Maintenance Department.
It is in fact a particular case of the long-term scheduled plant shut-down and the
same procedure explained in Section 6.7.1.2 will be followed, with the only
exception that, in this case, the raw materials contained in the plant feeding bins will
be emptied as well. In the previous case, this emptying will only take place at the
plant Director discretion, and might not be compulsory depending on the length of
the shutdown and the type of raw material contained.
When the plant is all empty, the annual cleanings and repairs will take place. Once
finished, the plant preparation and start-up operations will be carried out according
to the already explained procedures.
6.7.2 Plant emergency shut-down
The plant interlocking system, detailed in section 2.3, will be carefully studied in
order to know it well. It shows that some equipment failure can cause an unexpected
plant emergency shut-down either complete or partial.
During these shut-downs, if the plant is expected to be re-started in 2-4 hours, the
12-D-311A/B 02-TK302/310 vessel % N and %P2O5 will have to be checked. If they
were high, the liquid might crystallize on cooling (consult tables). Thus, it is
important to keep the scrubbing system in recirculation even with the agitator in
operation, and occasionally add water and/or fresh phosacid (diluted or
concentrated) to increase the salts solubility and/or reduce the molar ratio N/P.
During any emergency shut-down the granulator will be turned round several times,
specially during the first minutes, in order to avoid the product solidifying inside it,
which could cause serious damage to the equipment on starting it. If there are some
solidifications, before the start-up they should be manually cleaned leaving all
internals free to move.
The ammonia injectors to the granulator solids bed will be cleaned with steam and
air, taking care in not wet the solids bed in excess, until the unit is restarted.
In case that the equipment accusing the emergency shut-down was not absolutely
necessary for the granulation loop operation, this can be kept in recirculation if the
shut-down is going to last for 0,5 hours maximum. If it lasted longer, it would be
damaging to the scrubbing liquids that, being in a closed circuit, would increase their
solids content. To lessen these effects, the inspection doors on the granulator
product exit side will be opened, decreasing the suction from the granulator solids
bed.
The main fan dampers will be partially closed and some water added to the
granulator's bed to avoid the product becoming too dry and the dust being easily
sucked by the fan. This will also help reduce product temperature in the dryer, due
to the vaporization of water from it.
Occasionally, and depending on the throughput characteristics, it can be tried to add

steam through the ammonia injectors, though controlling the quantity added, to
avoid pasting the solids bed.
6.7.3 Plant shut-down due to electrical power failure
In this case all the plant equipment will be stopped and the following measures will
be taken:
1. Close ammonia feed to plant at B.L.
2. Close phosphoric acid and sulphuric acid fed to plant at B.L.
3. Add steam and additionally water to dilute slurry to PN through the ammonia
injectors.
4. Drain slurry transfer lines from PN to granulator and flush them with steam.
5. Clean the PRs with steam, manually through the by-pass valve. Clean, if
possible, ammonia spargers.
6. If the steam is expected to fail as well (shut-down over 30-45 min.) the PN will
be drained and the slurry diluted with water before it becomes too cold inside
the PN. Drainages will go to the sump tank for its later recovery.
7. Before re-starting the plant check lower parts of the elevators and clean them.
8. Break product build-ups inside the granulator and mechanically clean the
ploughshares ends before re-starting the plant.
6.8 CHANGE IN PRODUCT MANUFACTURE
The procedure to carry on the change in product manufacture depends basically on

three points:
a) Washing liquid in the scrubbing system
If the new product to be manufactured has to use phosacid concentration level

similar to the previous one (change from DAP to NPK, or from NPK to NPK), is
not necessary to adjust the liquid concentration in the scrubbing system but if not
(change from DAP/NPK to SAB NPKs like15-15-15 or vice versa), it is obvious
that the scrubbing liquids and also the phosacid liquor in PR vessel 02-TK-301
will have to be diluted or concentrated accordingly, by feeding fresh phosacid or
even process water if required to each mentioned vessels.
To adjust the washing acid concentration the plant will be stopped using the
normal shut-down procedure, but without emptying vessels (to keep 30-40% level
in each vessel is usually enough), and, after this, the vessels 02-TK-310, 02-TK-
301 and 12-D-311A/B, must be re-filled as explained above. From actual
concentration and vessel level is not difficult to calculate the quantities of acid or
water to be fed in order to obtain the desirable concentration for the new product
to be manufactured.
b) Differences on the used process
According to the plant design, two type of processes will be used :

- Mixed PN & PR process, where preneutralizer will be kept in operation.
- Single PR process, where preneutralizer will not be kept in operation.
So, depending on the process to be used for the next grade manufacture, the
preneutralizer will be taken into account to realize the corresponding change :
If the change is from mixed PN&PR process to single PR process, the

preneutralizer has to be emptied, as indicated in 6.7.1.2, before finishing the
production of the previous grade.
If the change is the opposite, from single PR process to mixed PN&PR process,
the preneutralizer has to be loaded, as indicated in 6.5.1, before starting the
production of the new grade.
If the change is from DAP to 15-15-15 (or NP with high sulphuric acid content) or
vice versa, both using mixed PN&PR process, preneutralizer level will be reduced
to a minimum before finishing the production of the previous grade and re-loaded
it with the appropriate slurry before starting the production of the new grade. A
compensatory feedings of ammonia and acid will be used taking into account the
amount of old slurry remaining in the PN and its analysis. As an alternative, the
PN can be completely emptied instead reducing its level and using a
compensatory feedings.
c) Differences between types / grades

If the new product to be manufactured has a similar composition that the one
which is being produced, it will be not necessary to change the seed, being
enough using a compensatory formulation during about few hours to transform
the analysis of the remaining product in the plant. If some "off-spec" product is
produced during the first hours of the new production, this product can be
segregated in stores in order to reprocess it to plant.
The procedure to carry on this kind of product change is based on the following
points:
- Stop the raw materials feedings and send all the product on size to
storage, till keeping in the granulation loop the minimum possible quantity
of product.
- After this, stop the plant and adjust the washing liquid concentration if
needed, as it has been explained before.
- Calculate the compensatory formulation that will be necessary to

introduce through the solid weighers and liquid flowmeters in order to
transform the analysis of the remaining product in the throughput.
- Start feedings of raw materials according to this compensatory

formulation, keeping stopped the recycle regulator belt conveyor, to have
the product in a closed circuit.
- The compensatory formulation has to be introduced for 1 hour typically.

After this time, open the final product extraction and set the normal
feeding flows for the new product, starting the normal process controls.
When the new product to be manufactured is very different from the previous
one, (for example, changing from DAP to NPK or vice versa) the plant has to be
completely emptied, sending the product to the seed room, being later filled with
the same or similar product to be manufactured, following the instructions given
in Section 6.5.1.
CHAPTER 7- PHYSICAL AND CHEMICAL DATA

CHAPTER 8- MASS & ENERGY BALANCES

Sheet 1 of 9
Incro , S.A. MASS & ENERGY BALANCE DAP 18-46-0 JOB N : REVISION 0
Rehabilitation and Flexible Operation PF-1 Plant DATE : October-2002 DATE ########
Petrokimia Gresik Pipe Reactor process BASIC ENGINEERING APPROVED J.R.
Stream number 100 101 102 104 120 121 122 123 124 125 140 141 142
Total Liquid Liquid Liquid Total Phosacid Phosacid Phosacid Phosacid Phosacid Total Sulphuric Sulphuric
Denomination liquid Ammonia Ammonia Ammonia Phosacid to to to to to Dust Sulphuric Acid to Acid
Ammonia to to P.Reactor to to P. Reactor Granulator Scrubber PN Scrubber Acid Granulator to
to Train Granulator "A" & "B" PN Plant Vessel Pre-Scrub. Vessel Vessel to Plant Pre-Scrub. PN
1. Flow units m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h
2. Design flow 25 8 10 14 40 12 30 8 12 2 20 4 15
3. Normal flow 18,1 5,2 7,0 0,0 34,4 6,35 23,9 3,3 0,0 0,85 0,09 0,0 0,0
4. Masic flow (kg/h) 12.257 3.331 4.463 0 55.407 10.250 38.511 5.261 0 1.385 171 0 0
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt 82,00 82,00 82,00 82,00 ** ** ** ** ** ** ** ** **
10. P2O5 Av. % wt ** ** ** ** 48,00 48,00 48,00 48,00 48,00 48,00 ** ** **
11. H2SO4 free % wt ** ** ** ** 2,88 2,88 2,88 2,88 2,88 2,88 98,00 98,00 98,00
12. K2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
13. H2O % wt 0,5 Max 0,5 Max 0,5 Max 0,5 Max 23,20 23,20 23,20 23,20 23,20 23,20 2,00 2,00 2,00
14. Solids % wt ** ** ** ** 3,0 3,0 3,0 3,0 3,0 3,0 ** ** **
15. Temperature C -30 0 0 0 33 33 33 33 33 33 33 33 33
16. Pressure (g) 10 4-6 6-8 4-6 5 5 5 5 5 5 4 4 4
Kg/cm2 (wc m.m)
17. Density 678 638 638 638 1610 1610 1610 1610 1610 1610 1840 1840 1840
Kg/m3 at T C
Minimum Flow Reactor Maximum Reactor Reactor
18. Remarks 9 Kg/cm2 to each not used 4% solids not used not used
P. Reactor
Sheet 2 of 9
Incro , S.A. MASS & ENERGY BALANCE DAP 18-46-0 JOB N : 0 REVISION 0
Stream number 143 144 145 210 230 240 280 290 310 311 312 313 320
Sulphuric Sulphuric Sulphuric Urea Potash Filler TSP/A.S. Micro- Total Plant Air Plant Air Plant Air Total
Denomination Acid Acid to Acid to to to to to nutrients Plant Air to clean to clean to Clarified
to Scrubber Tail Gas process process process process or A.S. to Ammonia Sulphuric RM Bins Water
Granulator Vessel Scrubber process sparger distributor Big Blasters to Plant
1. Flow units m3/h m3/h l/h t/h t/h t/h t/h t/h kg/h kg/h kg/h kg/h m3/h
2. Design flow 2 2 300 30 30 15 35 10 300 60 40 150 40
3. Normal flow 0,0 0,0 90 0,0 0,0 0,0 0,0 1,3 30-80 1-10 1-10 20-40 10,3
4. Masic flow (kg/h) 0 0 171 0 0 0 0 1.300 30-80 1-10 1-10 20-40 10.270
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt ** ** ** 46,00 ** ** ** 21,00 ** ** ** ** **
10. P2O5 Av. % wt ** ** ** ** ** ** ** ** ** ** ** ** **
11. H2SO4 free % wt 98,00 98,00 98,00 ** ** ** ** ** ** ** ** ** **
12. K2O % wt ** ** ** ** 60,00 ** ** ** ** ** ** ** **
13. H2O % wt 2,00 2,00 2,00 0,50 1,00 ** ** 0,15 ** ** ** ** 100,00
14. Solids % wt ** ** ** 99,5 99,0 ** ** 99,85 ** ** ** ** **
15. Temperature C 33 33 33 33 33 33 33 33 25 25 25 25 32
16. Pressure (g) 4 4 4 Grav. Grav. Grav. Grav. Grav. 5 4,5 4,5 4,5 2,5
Kg/cm2 (wc m.m)
17. Density 1840 1840 1840 800 1300 1000-1300 900-1100 1050 6,5 6,5 6,5 6,5 995
Kg/m3 at T C
Through Prill Minimum Am. Sulphate Including Only for Only for
18. Remarks pH 90% Minimum small flushing flushing
controller 0.15-1.2 mm 90% users eventually eventually
0.15-1.2 mm
Sheet 3 of 9
Stream number 321 322 323 324 326 330 340 350 360 362 363 370 371
Clarified Clarified Clarified Clarified Clarified Coating Coating Defoamer Total LP Steam LP Steam Total MP Steam
Denomination Water to Water to Water to Water to Water to 2nd Oil Powder to LP Steam to Cooler to MP Steam to
P. Reactor Scrubber Granulator Tail Gas GTSP/DAP to to Washing to Air Heater Dedusting to P.Reactor
Vessel Vessel Pre-Scrub. Scrubber Reactor(PN) Coater Coater System Plant E-304 Air Heater Plant (A/B)
1. Flow units m3/h m3/h m3/h m3/h m3/h l/h kg/h l/h kg/h kg/h kg/h kg/h kg/h
2. Design flow 2 2 2 30 8 300 500 150 1.100 400 500 3.000 2.500
3. Normal flow 0,0 0,0 0,0 10,3 0,0 0,0 0,0 10-30 450 150 300 80-115 70-100
4. Masic flow (kg/h) 0 0 0 10.270 0 0 0 8-25 450 150 300 80-115 70-100
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt ** ** ** ** ** ** ** ** ** ** ** ** **
10. P2O5 Av. % wt ** ** ** ** ** ** ** ** ** ** ** ** **
11. H2SO4 free % wt ** ** ** ** ** ** ** ** ** ** ** ** **
12. K2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
13. H2O % wt 100,00 100,00 100,00 100,00 100,00 ** 0,50 ** 100,00 100,00 100,00 100,00 100,00
14. Solids % wt ** ** ** ** ** ** 99,5 ** ** ** ** ** **
15. Temperature C 32 32 32 32 32 70-80 33 33 158 158 158 170 170
16. Pressure (g) 2,5 2,5 2,5 2,5 2,5 4,0 Grav. 3 5 5 5 7 7
Kg/cm2 (wc m.m)
17. Density 995 995 995 995 995 880 500 900 3,05 3,05 3,05 3,96 3,96
Kg/m3 at T C 930 at 15C bulk density
Used Used Used Used Normally Normally Feed to : Minimum Alternativelly
18. Remarks only only only only not used not used S-801 pressure to each PR
eventually eventually eventually eventually for DAP for DAP C-302 for flushing for flushing
T-301 7 k/cm2 g at 2.5 t/h
Sheet 4 of 9
Stream number 372 380 390 400 401 402 404 410 411 412 413 414 420
MP Steam Natural Gas Total Total Granulator Dryer Solids to Fines Oversizes Onsize Recycle Onsize Onsize
Denomination to to LP Conden. Solids discharge discharge Screens to to Mills Product to regulator Product to Product
Ammonia Dryer to B.L. to to to Distributors Recycle & Recycle Recycle overflow Collector to
sparger Burner Granulator Dryer Conveyor (2 lines) (4 lines) (4 lines) regulator to Recycle (4 lines) Cooler
1. Flow units kg/h Mkcal/h kg/h t/h t/h t/h t/h t/h t/h t/h t/h t/h t/h
2. Design flow 1.000 EXISTING 1.100 390 390 390 200 50 40 300 300 75 100
3. Normal flow 10-15 2.600 450 275 334 329,0 164,5 16,4 20,6 181,0 122,4 45,3 58,6
4. Masic flow (kg/h) 10-15 ** 450 274.840 334.287 329.020 164.510 16.400 20.600 181.020 122.420 45.255 58.600
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt ** ** ** 18,11 17,99 18,10 18,10 18,10 18,10 18,10 18,10 18,10 18,10
10. P2O5 Av. % wt ** ** ** 45,88 45,73 46,10 46,10 46,10 46,10 46,10 46,10 46,10 46,10
11. H2SO4 free % wt ** ** ** ** ** ** ** ** ** ** ** ** **
12. K2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
13. H2O % wt 100,00 ** 100,00 1,29 2,10 1,30 1,30 1,30 1,30 1,30 1,30 1,30 1,30
14. Solids % wt ** ** ** 98,7 97,9 98,7 98,7 98,7 98,7 98,7 98,7 98,7 98,7
15. Temperature C 170 33 100-158 85 105 99 95 90 90 88 88 88 86
16. Pressure (g) 7 25-40 5 Grav. Grav. Grav. Grav. Grav. Grav. Grav. Grav. Grav. Grav.
Kg/cm2 (wc m.m)
17. Density 3,96 by GRESIK 959 1050 1000 1000 1000 1050 940/1070 1000 1000 1000 1000
Kg/m3 at T C bulk density bulk density bulk density bulk density bulk density bulk density bulk density bulk density bulk density bulk density
Eventual Calorific Granulom. Granulom. Granulom. Flow for Flow for Flow for Flow for Cooler with
18. Remarks flushings value: >4 = 7% >4 = 20% >4 = 20% each line each line each line each line chilled air
of 1.5 t/h 4-2= 55% 4-2= 66% 4-2= 66% (A/B) (A/B/C/D) (A/B/C/D) (A/B/C/D) to reach
Kcal/Nm3 <2 = 38% <2 = 14% <2 = 14% 46C
Sheet 5 of 9
Stream number 440 441 442 450 480 490 491 492 500 501 502 503 505
Onsize Fines+Ov Onsize Final Recyle Dust from Dust from Dust from Gases Gases Total Gases from Gases
Denomination Product f/ polishing Product Product to Dryer Cooler Dedusting from PN from GRAN Gases Pre-Scrub. from
to polishing Screen to to Granulator Cyclones Cyclones Cyclones to to to to Gran Gran Scrub.
Screen to Recycle Coater Storage to Recycle to Recycle to Recycle Pre-Scrub. Pre-Scrub. Pre-Scrub. Scrubber to TGS
1. Flow units t/h t/h t/h t/h t/h t/h t/h t/h Am3/h Am3/h Am3/h Am3/h Am3/h
2. Design flow 100 20 90 90 390 5 1,5 4 45.000 85.000 85.000 90.000 80.000
3. Normal flow 58,2 1,2 57,0 57,0 273,5 2,0 0,3 1,6 0 74.435 74.435 79.560 70.925
4. Masic flow (kg/h) 58.200 1.200 57.000 57.000 273.540 2.000 320 1.600 0 66.591 66.591 66.095 63.112
5. Dry air (kg/h) ** ** ** ** ** ** ** ** 0 49.000 49.000 49.000 49.000
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** 0 90 90 43 77
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** 0 27.715 27.715 3.896 606
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** 0 13.435 13.435 1.257 141
9. N % wt 18,10 18,10 18,10 18,10 18,10 18,10 18,10 18,10 ** ** ** ** **
10. P2O5 Av. % wt 46,10 46,10 46,10 46,10 46,10 46,10 46,10 46,10 ** ** ** ** **
11. H2SO4 free % wt ** ** ** ** ** ** ** ** ** ** ** ** **
12. K2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
13. H2O % wt 1,30 1,30 1,30 1,30 1,30 1,30 1,30 1,30 ** ** ** ** **
14. Solids % wt 98,7 98,7 98,7 98,7 98,7 98,7 98,7 98,7 ** ** ** ** **
15. Temperature C 46 86 46 45 86 95 60 44 ** 73,5 73,5 95 76,5
16. Pressure (g) Grav. Grav. Grav. Grav. Grav. Grav. Grav. Grav. (- 50) (- 50) (- 70) (- 220) (-500/+250)
Kg/cm2 (wc m.m)
17. Density 1000 1000 1000 1000 1020 1080 1080 1080 ** 0,895 0,895 0,831 0,890
Kg/m3 at T C bulk density bulk density bulk density bulk density bulk density bulk density bulk density bulk density
Product Granulom. Granulom. Reactor T max. T max. T max.
18. Remarks not coated 4-2=90% >4 = 7% not used 85C 90C 100C Fluorine
4-1=95% 4-2= 55% 170-200 ppm
<1=1% <2 = 38%
Sheet 6 of 9
Stream number 510 511 512 513 515 516 517 518 519 520 521 522 523
Combustion Quench Recirc. Air Gases Gases Gases Fumes Total Fumes Air from Air from Gases Fresh Air
Denomination Air to Air to from Cooler from Dryer to from Dryer from TSP-2 gases from TSP-2 Dedusting Dedusting from Dust to Dedust.
Dryer Dryer Cyclones to Dryer Dryer Scrubber to recirculated to system to Cyclones to Scrubber heating
Burner Burner to Dryer Cyclones Scrubber to TGS Dryer Scr. to Dryer Pre-Scrub. Cyclones Dust Scrub. to TGS system
1. Flow units Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h
2. Design flow EXISTING EXISTING 75.000 150.000 150.000 150.000 GRESIK 75.000 GRESIK 78.000 78.000 78.000 10.000
3. Normal flow 4.035 40.790 74.540 143.370 142.600 135.900 0 74.540 0 73.480 73.250 72.285 9.000
4. Masic flow (kg/h) 4.599 46.501 78.435 135.400 133.400 138.751 0 78.435 0 82.492 80.892 81.657 10.260
5. Dry air (kg/h) 4.500 45.500 77.500 127.500 127.500 127.500 0 77.500 0 79.000 79.000 79.000 10.040
6. Rel. Humidity (%) 70 70 8,4 6,4 6,9 72 ** 8,4 ** 29 30 95 70
7. NH3 in air (mg/Am3) 0 0 27 1.046 1.052 133 ** 27 ** 680 683 69 0
8. Dust in air (mg/Am3) 0 0 1.073 17.437 3.506 368 ** 1.073 ** 27.218 5.461 553 0
9. N % wt ** ** ** ** ** ** ** ** ** ** ** ** **
10. P2O5 Av. % wt ** ** ** ** ** ** ** ** ** ** ** ** **
11. H2SO4 free % wt ** ** ** ** ** ** ** ** ** ** ** ** **
12. K2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
13. H2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
14. Solids % wt ** ** ** ** ** ** ** ** ** ** ** ** **
15. Temperature C 33 33 61 99 97 57 ** 61 ** 46 45 34 33
16. Pressure (g) by GRESIK by GRESIK (-150/+80) (- 50) (- 175) (-450/+250) ** (-150/+80) ** (- 120) (- 200) (-600/+250) (-25/+200)
Kg/cm2 (wc m.m)
17. Density 1,140 1,140 1,052 0,944 0,936 1,021 ** 1,052 ** 1,123 1,104 1,130 1,140
Kg/m3 at T C
Ambient Ambient T max. Line Line Ambient
18. Remarks air air 110C Fluorine not used not used Fluorine air
55-75 ppm 15-20 ppm
Sheet 7 of 9
Stream number 524 530 543 544 545 550 551 600 601 602 603 604 605
Heated Gases Ambient Chilled Air Desaturated Total Gases Washing Washing Washing Liq.Transfer Liquid Liquid
Denomination Air to from Cooler Air to to Cooler Air Gases from TGS liquid to liquid to liquid to from TGS from TGS to from TGS
Dedusting to Cooler Cooler Air to to to TGS 1st step 2nd step to Dust Scr. GTSP/DAP to
system Cyclones Air Chiller Heater Cooler TGS ATM inlet duct TGS TGS Vessel Reactor(PN) Granulator
1. Flow units Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h m3/h m3/h m3/h m3/h m3/h m3/h
2. Design flow 12.000 75.000 70.000 70.000 70.000 300.000 300.000 600 300 300 30 10 5
3. Normal flow 10.820 74.760 69.500 64.800 65.400 279.110 277.430 559,1 285,0 267,9 10,9 0,0 0,0
4. Masic flow (kg/h) 10.260 78.755 79.236 78.353 78.353 283.520 283.042 557.980 281.295 264.149 10.916 0 0
5. Dry air (kg/h) 10.040 77.500 77.500 77.500 77.500 255.500 255.500 ** ** ** ** ** **
6. Rel. Humidity (%) 4,0 8,0 70 100 75 91 100 ** ** ** ** ** **
7. NH3 in air (mg/Am3) 0 27 0 0 0 236 28 ppm ** ** ** ** ** **
8. Dust in air (mg/Am3) 0 5.350 0 0 0 358 35 ppm ** ** ** ** ** **
9. N % wt ** ** ** ** ** ** ** 0,58 0,14 0,06 0,58 ** **
10. P2O5 Av. % wt ** ** ** ** ** ** ** 0,38 0,22 0,09 0,38 ** **
11. H2SO4 free % wt ** ** ** ** ** ** ** 0,00 0,00 0,00 0,00 ** **
12. K2O % wt ** ** ** ** ** ** ** 0,00 0,00 0,00 0,00 ** **
13. H2O % wt ** ** ** ** ** ** ** 97,10 99,46 99,77 97,10 ** **
14. Solids % wt ** ** ** ** ** ** ** 1 max. 1 max. 1 max. 1 max. ** **
15. Temperature C 95 62 33 16 20 56,5 54 54,5 54 53 54,5 ** **
16. Pressure (g) (+ 150) (- 50) Atm by Vendor by Vendor (+ 200) (+ 50) 3 3 3 3 ** **
Kg/cm2 (wc m.m)
17. Density 0,948 1,053 1,140 1,217 1,198 1,016 1,020 998 987 986 998 980-1030 980-1030
Kg/m3 at T C
Used Chiller Condensed pH= 5.5 pH= 5.5 Reactor Normally
18. Remarks capacity water from Fluorine Fluorine not used not used
891.000 Chiller 70-80 ppm 4 ppm T max. T max. T max. T max. T max. T max.
Fr/h 883 k/h 60C 60C 60C 60C 60C 60C
Sheet 8 of 9
Stream number 606 607 620 621 630 632 635 640 645 660 661 662 663
Liquid Liquid Total flow Liq.Transfer Washing Washing Liquid Washing Liquid Total flow Liq.Transfer Liq.Transfer Total
Denomination from TGS to TGS of from Scrub. liquor to liquor to discharge liquor to discharge of from Pre- from Pre- washing
to Amm. from Amm. Scrubber Vessel to Gr. Scrub. Gran. Scr. from Gran. Dryer Scr. from Dryer Pre-Scrub. Scrub. to Scrub. to liquor to
Heater Heater Pump Pre-Scrub. + tranfer Arm Scrubber Arm Scrubber Pump PR Vessel PN Pre-Scrub.
2. Design flow 100 100 230 35 105 80 210 150 375 250 55 40 170
3. Normal flow 60,1 60,1 221,0 11,0 86,0 75,0 197,7 135,0 345,1 240,0 36,0 0,0 160,0
4. Masic flow (kg/h) 60.000 60.000 287.277 14.277 111.777 97.500 256.483 175.500 450.949 355.196 53.276 0 236.800
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt 0,58 0,58 4,15 4,15 4,15 4,15 4,19 4,15 4,24 4,12 4,12 ** 4,12
10. P2O5 Av. % wt 0,38 0,38 25,58 25,58 25,58 25,58 25,30 25,58 25,93 42,33 42,33 ** 42,33
11. H2SO4 free % wt 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 ** 0,00
12. K2O % wt 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 ** 0,00
13. H2O % wt 97,10 97,10 53,72 53,72 53,72 53,72 54,12 53,72 53,04 27,12 27,12 ** 27,12
14. Solids % wt 1 max. 1 max. 6 max. 6 max. 6 max. 6 max. 6 max. 6 max. 6 max. 10 max. 10 max. ** 10 max.
15. Temperature C 54,5 44,5 63 63 63 63 77 63 56 87,5 87,5 ** 87,5
16. Pressure (g) 3 3 3 3 3 3 Grav. 3 Grav. 4 4 ** 4
Kg/cm2 (wc m.m)
17. Density 998 999 1300 1300 1300 1300 1297 1300 1307 1480 1480 ** 1480
Kg/m3 at T C
pH= 5.5 pH= 5.5 N/P=0,77 N/P=0,77 N/P=0,77 N/P=0,77 N/P=0,79 N/P=0,77 N/P=0,78 N/P=0,42 N/P=0,42 Reactor N/P=0,42
18. Remarks not used
T max. T max. T max. T max. T max. T max. T max. T max. T max. T max. T max. T max.
60C 60C 75C 75C 75C 75C 85C 75C 75C 100C 100C 100C
Sheet 9 of 9
Stream number 666 670 680 681 682 690 691 692 695 700 710
Washing Phosacid Total flow Washing Washing Washing Washing Liq.Transfer Liquid Discharge Discharge
Denomination liquor to liquor to of 02-P-302 liquor to liquor to liquor to liquor to from Dust discharge PR slurry PN slurry
Pre-Scrub. P. Reactor A/B Gran. Scr. Dryer Scr. Dust Scr. Dust Scr. Scrub. to from Dust "A" & "B" to to
Duct "A" & "B" Ventury Ventury Ventury Arm Scr.Vessel Scrubber Granulator Granulator
1. Flow units m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h t/h m3/h
2. Design flow 50 30 2 x 175 125 225 102 146 30 248 40 40
3. Normal flow 44,0 21,2 336,0 120,0 216,0 98,0 131,6 8,6 228,4 30,0 0,0
4. Masic flow (kg/h) 65.120 31.763 415.296 156.000 280.800 110.740 148.708 9.752 258.683 30.001 0
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** **
9. N % wt 4,12 3,46 3,61 4,15 4,15 1,01 1,01 1,01 1,05 14,02 **
10. P2O5 Av. % wt 42,33 43,24 22,22 25,58 25,58 7,54 7,54 7,54 7,63 45,78 **
11. H2SO4 free % wt 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 **
12. K2O % wt 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 **
13. H2O % wt 27,12 26,49 62,43 53,72 53,72 86,56 86,56 86,56 86,36 9,58 **
14. Solids % wt 10 max. 10 max. 6 max. 6 max. 6 max. 4 max. 4 max. 4 max. 4 max. 90,4 **
15. Temperature C 87,5 80 63 63 63 33 33 33 32 135-140 **
16. Pressure (g) 4 3-7 3 3 3 3 3 3 Grav 2 **
Kg/cm2 (wc m.m)
17. Density 1480 1500 1236 1300 1300 1130 1130 1130 1133 1550 **
Kg/m3 at T C
N/P=0,42 N/P=0,33 N/P=0,77 N/P=0,77 N/P=0,77 N/P=0,64 N/P=0,64 N/P=0,64 N/P=0,67 N/P = 1,47 Reactor
18. Remarks Flow to Tmax 155C not used
T max. each PR Two pumps T max. T max. T max. T max. T max. T max. Flow from
100C in service 75C 75C 45C 45C 45C 45C each PR
Sheet 1 of 9
Incro , S.A. MASS & ENERGY BALANCE NPK 15-15-15 JOB N : REVISION 0
Petrokimia Gresik Mixed process Reactor / Pipe Reactor - Sulphuric basis BASIC ENGINEERING APPROVED J.R.
Stream number 100 101 102 104 120 121 122 123 124 125 140 141 142
Total Liquid Liquid Liquid Total Phosacid Phosacid Phosacid Phosacid Phosacid Total Sulphuric Sulphuric
Denomination liquid Ammonia Ammonia Ammonia Phosacid to to to to to Dust Sulphuric Acid to Acid
Ammonia to to P.Reactor to to P. Reactor Granulator Scrubber PN Scrubber Acid Granulator to
to Train Granulator "A" or "B" PN Plant Vessel Pre-Scrub. Vessel Vessel to Plant Pre-Scrub. PN
2. Design flow 25 8 10 14 40 12 30 8 12 2 20 4 15
3. Normal flow 15,5 4,35 2,45 9,6 11,7 4,45 4,6 2,2 0,0 0,45 10,2 2,45 6,95
4. Masic flow (kg/h) 10.480 2.784 1.570 6.126 18.879 7.174 7.457 3.493 0 755 18.768 4.504 12.810
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt 82,00 82,00 82,00 82,00 ** ** ** ** ** ** ** ** **
10. P2O5 Av. % wt ** ** ** ** 48,00 48,00 48,00 48,00 48,00 48,00 ** ** **
11. H2SO4 free % wt ** ** ** ** 2,88 2,88 2,88 2,88 2,88 2,88 98,00 98,00 98,00
12. K2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
13. H2O % wt 0,5 Max 0,5 Max 0,5 Max 0,5 Max 23,20 23,20 23,20 23,20 23,20 23,20 2,00 2,00 2,00
14. Solids % wt ** ** ** ** 3,0 3,0 3,0 3,0 3,0 3,0 ** ** **
15. Temperature C -30 0 0 0 33 33 33 33 33 33 33 33 33
16. Pressure (g) 10 4-6 6-8 4-6 5 5 5 5 5 5 4 4 4
Kg/cm2 (wc m.m)
17. Density 678 638 638 638 1610 1610 1610 1610 1610 1610 1840 1840 1840
Kg/m3 at T C
Minimum Flow Maximum
18. Remarks 9 Kg/cm2 to one 4% solids
P. Reactor
Sheet 2 of 9
Incro , S.A. MASS & ENERGY BALANCE NPK 15-15-15 JOB N : 0 REVISION 0
Stream number 143 144 145 210 230 240 280 290 310 311 312 313 320
Sulphuric Sulphuric Sulphuric Urea Potash Filler TSP/A.S. Micro- Total Plant Air Plant Air Plant Air Total
Denomination Acid Acid to Acid to to to to to nutrients Plant Air to clean to clean to Clarified
to Scrubber Tail Gas process process process process or A.S. to Ammonia Sulphuric RM Bins Water
Granulator Vessel Scrubber process sparger distributor Big Blasters to Plant
1. Flow units m3/h m3/h l/h t/h t/h t/h t/h t/h kg/h kg/h kg/h kg/h m3/h
2. Design flow 2 2 300 30 30 15 35 10 300 60 40 150 40
3. Normal flow 0,7 0,0 86 0,9 15,0 0,0 0,0 0,0 30-80 1-10 1-10 20-40 20,1
4. Masic flow (kg/h) 1.295 0 159 900 15.003 0 0 0 30-80 1-10 1-10 20-40 19.960
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt ** ** ** 46,00 ** ** ** 21,00 ** ** ** ** **
10. P2O5 Av. % wt ** ** ** ** ** ** ** ** ** ** ** ** **
11. H2SO4 free % wt 98,00 98,00 98,00 ** ** ** ** ** ** ** ** ** **
12. K2O % wt ** ** ** ** 60,00 ** ** ** ** ** ** ** **
13. H2O % wt 2,00 2,00 2,00 0,50 1,00 ** ** 0,15 ** ** ** ** 100,00
14. Solids % wt ** ** ** 99,5 99,0 ** ** 99,85 ** ** ** ** **
15. Temperature C 33 33 33 33 33 33 33 33 25 25 25 25 32
16. Pressure (g) 4 4 4 Grav. Grav. Grav. Grav. Grav. 5 4,5 4,5 4,5 2,5
Kg/cm2 (wc m.m)
17. Density 1840 1840 1840 800 1300 1000-1300 900-1100 1050 6,5 6,5 6,5 6,5 995
Kg/m3 at T C
Through Prill Minimum Am. Sulphate Including Only for Only for
18. Remarks pH 90% Minimum small flushing flushing
controller 0.15-1.2 mm 90% users eventually eventually
0.15-1.2 mm
Sheet 3 of 9
Stream number 321 322 323 324 326 330 340 350 360 362 363 370 371
Clarified Clarified Clarified Clarified Clarified Coating Coating Defoamer Total LP Steam LP Steam Total MP Steam
Denomination Water to Water to Water to Water to Water to 2nd Oil Powder to LP Steam to Cooler to MP Steam to
P. Reactor Scrubber Granulator Tail Gas GTSP/DAP to to Washing to Air Heater Dedusting to P.Reactor
Vessel Vessel Pre-Scrub. Scrubber Reactor(PN) Coater Coater System Plant E-304 Air Heater Plant (A/B)
1. Flow units m3/h m3/h m3/h m3/h m3/h l/h kg/h l/h kg/h kg/h kg/h kg/h kg/h
2. Design flow 2 2 2 30 8 300 500 150 1.100 400 500 3.000 2.500
3. Normal flow 0,0 0,0 0,0 20,1 0,0 68 240 10-30 480 180 300 60-85 50-70
4. Masic flow (kg/h) 0 0 0 19.960 0 60 240 8-25 480 180 300 60-85 50-70
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt ** ** ** ** ** ** ** ** ** ** ** ** **
10. P2O5 Av. % wt ** ** ** ** ** ** ** ** ** ** ** ** **
11. H2SO4 free % wt ** ** ** ** ** ** ** ** ** ** ** ** **
12. K2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
13. H2O % wt 100,00 100,00 100,00 100,00 100,00 ** 0,50 ** 100,00 100,00 100,00 100,00 100,00
14. Solids % wt ** ** ** ** ** ** 99,5 ** ** ** ** ** **
15. Temperature C 32 32 32 32 32 70-80 33 33 158 158 158 170 170
16. Pressure (g) 2,5 2,5 2,5 2,5 2,5 4,0 Grav. 3 5 5 5 7 7
Kg/cm2 (wc m.m)
17. Density 995 995 995 995 995 880 500 900 3,05 3,05 3,05 3,96 3,96
Kg/m3 at T C 930 at 15C bulk density
Used Used Used Used Feed to : Minimum To PR in
18. Remarks only only only only S-801 pressure operation
eventually eventually eventually eventually C-302 for flushing for flushing
T-301 7 k/cm2 g at 2.5 t/h
Sheet 4 of 9
Stream number 372 380 390 400 401 402 404 410 411 412 413 414 420
MP Steam Natural Gas Total Total Granulator Dryer Solids to Fines Oversizes Onsize Recycle Onsize Onsize
Denomination to to LP Conden. Solids discharge discharge Screens to to Mills Product to regulator Product to Product
Ammonia Dryer to B.L. to to to Distributors Recycle & Recycle Recycle overflow Collector to
sparger Burner Granulator Dryer Conveyor (2 lines) (4 lines) (4 lines) regulator to Recycle (4 lines) Cooler
1. Flow units kg/h Mkcal/h kg/h t/h t/h t/h t/h t/h t/h t/h t/h t/h t/h
2. Design flow 1.000 EXISTING 1.100 390 390 390 200 50 40 300 300 75 100
3. Normal flow 10-15 2.700 480 266,5 314,4 308,5 154,3 20,1 20,8 144,9 81,9 36,2 63,0
4. Masic flow (kg/h) 10-15 ** 480 266.483 314.400 308.500 154.250 20.100 20.800 144.900 81.900 36.225 63.000
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt ** ** ** 14,26 14,97 15,08 15,08 15,08 15,08 15,08 15,08 15,08 15,08
10. P2O5 Av. % wt ** ** ** 14,10 14,94 15,08 15,08 15,08 15,08 15,08 15,08 15,08 15,08
11. H2SO4 free % wt ** ** ** 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00
12. K2O % wt ** ** ** 17,48 14,94 15,08 15,08 15,08 15,08 15,08 15,08 15,08 15,08
13. H2O % wt 100,00 ** 100,00 1,00 1,90 1,00 1,00 1,00 1,00 1,00 1,00 1,00 1,00
14. Solids % wt ** ** ** 99,0 98,1 99,0 99,0 99,0 99,0 99,0 99,0 99,0 99,0
15. Temperature C 170 33 100-158 83 107 99 95 90 90 88 88 88 86
16. Pressure (g) 7 25-40 5 Grav. Grav. Grav. Grav. Grav. Grav. Grav. Grav. Grav. Grav.
Kg/cm2 (wc m.m)
17. Density 3,96 by GRESIK 959 1070 1020 1020 1020 1070 970/1100 1020 1020 1020 1020
Kg/m3 at T C bulk density bulk density bulk density bulk density bulk density bulk density bulk density bulk density bulk density bulk density
Eventual Calorific Granulom. Granulom. Granulom. Flow for Flow for Flow for Flow for Cooler with
18. Remarks flushings value: >4 = 7% >4 = 18% >4 = 18% each line each line each line each line chilled air
of 1.5 t/h 4-2= 42% 4-2= 62% 4-2= 62% (A/B) (A/B/C/D) (A/B/C/D) (A/B/C/D) to reach
Kcal/Nm3 <2 = 51% <2 = 20% <2 = 20% 46C
Sheet 5 of 9
Stream number 440 441 442 450 480 490 491 492 500 501 502 503 505
Onsize Fines/Ov. Onsize Final Recyle Dust from Dust from Dust from Gases Gases Total Gases from Gases
Denomination Product f/ polishing Product Product to Dryer Cooler Dedusting from PN from GRAN Gases Pre-Scrub. from
to polishing Screen to to Granulator Cyclones Cyclones Cyclones to to to to Gran Gran Scrub.
Screen to Recycle Coater Storage to Recycle to Recycle to Recycle Pre-Scrub. Pre-Scrub. Pre-Scrub. Scrubber to TGS
1. Flow units t/h t/h t/h t/h t/h t/h t/h t/h Am3/h Am3/h Am3/h Am3/h Am3/h
2. Design flow 100 20 90 90 390 5 1,5 4 45.000 85.000 85.000 90.000 80.000
3. Normal flow 62,4 2,7 59,7 60,0 250,6 2,4 0,5 2,0 33.350 41.590 74.940 82.860 74.590
4. Masic flow (kg/h) 62.400 2.700 59.700 60.000 250.580 2.400 480 2.000 26.417 42.094 68.511 70.654 66.577
5. Dry air (kg/h) ** ** ** ** ** ** ** ** 15.500 35.500 51.000 51.000 51.000
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** 100 90 100 74 90
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** 34.753 20.293 26.728 3.621 563
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** 0 28.853 16.013 1.448 161
9. N % wt 15,08 15,08 15,08 15,00 15,08 15,08 15,08 15,08 ** ** ** ** **
10. P2O5 Av. % wt 15,08 15,08 15,08 15,00 15,08 15,08 15,08 15,08 ** ** ** ** **
11. H2SO4 free % wt 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 ** ** ** ** **
12. K2O % wt 15,08 15,08 15,08 15,00 15,08 15,08 15,08 15,08 ** ** ** ** **
13. H2O % wt 1,00 1,00 1,00 1,00 1,00 1,00 1,00 1,00 ** ** ** ** **
14. Solids % wt 99,0 99,0 99,0 99,0 99,0 99,0 99,0 99,0 ** ** ** ** **
15. Temperature C 46 86 46 45 87 96 60 44 82 59 70 82 73,5
16. Pressure (g) Grav. Grav. Grav. Grav. Grav. Grav. Grav. Grav. (- 50) (- 50) (- 70) (-220) (-500/+250)
Kg/cm2 (wc m.m)
17. Density 1020 1020 1020 1020 1050 1100 1100 1100 0,792 1,012 0,914 0,853 0,893
Kg/m3 at T C bulk density bulk density bulk density bulk density bulk density bulk density bulk density bulk density
Granulom. Granulom. T max. T max. T max. T max.
18. Remarks 4-2=90% >4 = 7% 90C 85C 90C 100C Fluorine
4-1=95% 4-2= 44% 140-180 ppm
<1=1% <2 = 48%
Sheet 6 of 9
Stream number 510 511 512 513 515 516 517 518 519 520 521 522 523
Combustion Quench Recirc. Air Gases Gases Gases Fumes Total Fumes Air from Air from Gases Fresh Air
Denomination Air to Air to from Cooler from Dryer to from Dryer from TSP-2 gases from TSP-2 Dedusting Dedusting from Dust to Dedust.
Dryer Dryer Cyclones to Dryer Dryer Scrubber to recirculated to system to Cyclones to Scrubber heating
Burner Burner to Dryer Cyclones Scrubber to TGS Dryer Scr. to Dryer Pre-Scrub. Cyclones Dust Scrub. to TGS system
1. Flow units Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h
2. Design flow EXISTING EXISTING 75.000 150.000 150.000 150.000 GRESIK 75.000 GRESIK 78.000 78.000 78.000 10.000
3. Normal flow 4.215 40.610 74.180 143.950 143.180 136.860 0 74.180 0 73.460 73.230 72.080 9.000
4. Masic flow (kg/h) 4.803 46.297 78.241 136.019 133.619 139.958 0 78.241 0 82.982 80.982 81.860 10.260
5. Dry air (kg/h) 4.700 45.300 77.500 127.500 127.500 127.500 0 77.500 0 79.000 79.000 79.000 10.040
6. Rel. Humidity (%) 70 70 6,1 6,4 6,9 87 ** 6,1 ** 29 30 97 70
7. NH3 in air (mg/Am3) 0 0 13 695 698 88 ** 13 ** 545 546 55 0
8. Dust in air (mg/Am3) 0 0 1.618 20.840 4.190 438 ** 1.618 ** 34.032 6.828 694 0
9. N % wt ** ** ** ** ** ** ** ** ** ** ** ** **
10. P2O5 Av. % wt ** ** ** ** ** ** ** ** ** ** ** ** **
11. H2SO4 free % wt ** ** ** ** ** ** ** ** ** ** ** ** **
12. K2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
13. H2O % wt ** ** ** ** ** ** ** ** ** ** ** ** **
14. Solids % wt ** ** ** ** ** ** ** ** ** ** ** ** **
15. Temperature C 33 33 61 100 98 55 ** 61 ** 46 45 35 33
16. Pressure (g) by GRESIK by GRESIK (-150/+80) (- 50) (- 175) (-450/+250) ** (-150/+80) ** (- 120) (- 200) (-600/+350) (-25/+200)
Kg/cm2 (wc m.m)
17. Density 1,140 1,140 1,055 0,945 0,933 1,023 ** 1,055 ** 1,130 1,106 1,136 1,140
Kg/m3 at T C
Ambient Ambient T max. Line Line Ambient
18. Remarks air air 110C Fluorine not used not used Fluorine air
55-75 ppm 5-10 ppm
Sheet 7 of 9
Stream number 524 530 543 544 545 550 551 600 601 602 603 604 605
Heated Gases Ambient Chilled Air Desaturated Total Gases Washing Washing Washing Liq.Transfer Liquid Liquid
Denomination Air to from Cooler Air to to Cooler Air Gases from TGS liquid to liquid to liquid to from TGS from TGS to from TGS
Dedusting to Cooler Cooler Air to to to TGS 1st step 2nd step to Dust Scr. GTSP/DAP to
system Cyclones Air Chiller Heater Cooler TGS ATM inlet duct TGS TGS Vessel Reactor(PN) Granulator
1. Flow units Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h Am3/h m3/h m3/h m3/h m3/h m3/h m3/h
2. Design flow 12.000 75.000 70.000 70.000 70.000 300.000 300.000 600 300 300 30 10 5
3. Normal flow 10.820 74.410 69.500 63.080 64.190 283.530 283.150 548,3 285,0 267,9 21,7 0,0 0,0
4. Masic flow (kg/h) 10.260 78.721 79.236 78.120 78.120 288.395 287.064 542.817 280.725 263.882 21.467 0 0
5. Dry air (kg/h) 10.040 77.500 77.500 77.500 77.500 257.500 257.500 ** ** ** ** ** **
6. Rel. Humidity (%) 4,0 5,8 70 100 70 98 100 ** ** ** ** ** **
7. NH3 in air (mg/Am3) 0 13 0 0 0 205 26 ppm ** ** ** ** ** **
8. Dust in air (mg/Am3) 0 8.063 0 0 0 430 40 ppm ** ** ** ** ** **
9. N % wt ** ** ** ** ** ** ** 0,27 0,07 0,03 0,27 ** **
10. P2O5 Av. % wt ** ** ** ** ** ** ** 0,08 0,04 0,02 0,08 ** **
11. H2SO4 free % wt ** ** ** ** ** ** ** 0,00 0,00 0,00 0,00 ** **
12. K2O % wt ** ** ** ** ** ** ** 0,08 0,04 0,02 0,08 ** **
13. H2O % wt ** ** ** ** ** ** ** 98,52 99,68 99,86 98,52 ** **
14. Solids % wt ** ** ** ** ** ** ** 1 max. 1 max. 1 max. 1 max. ** **
15. Temperature C 95 62 33 11 16 56 55 55,5 55 53,5 55,5 ** **
16. Pressure (g) (+ 150) (- 50) Atm by Vendor by Vendor (+ 200) (+ 50) 3 3 3 3 ** **
Kg/cm2 (wc m.m)
17. Density 0,948 1,058 1,140 1,238 1,219 1,017 1,014 990 985 985 990 980-1030 980-1030
Kg/m3 at T C
Used Chiller Condensed pH= 5.5 pH= 5.5 Used Normally
18. Remarks capacity water from Fluorine Fluorine eventually not used
1.105.000 Chiller 55-70 ppm 4 ppm T max. T max. T max. T max. T max. T max.
Fr/h 1116 k/h 60C 60C 60C 60C 60C 60C
Sheet 8 of 9
Stream number 606 607 620 621 630 632 635 640 645 660 661 662 663
Liquid Liquid Total flow Liq.Transfer Washing Washing Liquid Washing Liquid Total flow Liq.Transfer Liq.Transfer Total
Denomination from TGS to TGS of from Scrub. liquor to liquor to discharge liquor to discharge of from Pre- from Pre- washing
to Amm. from Amm. Scrubber Vessel to Gr. Scrub. Gran. Scr. from Gran. Dryer Scr. from Dryer Pre-Scrub. Scrub. to Scrub. to liquor to
Heater Heater Pump Pre-Scrub. + tranfer Arm Scrubber Arm Scrubber Pump PR Vessel PN Pre-Scrub.
2. Design flow 100 100 270 35 105 80 210 150 375 250 55 40 170
3. Normal flow 60,6 60,5 221,0 19,3 91,0 71,7 195,5 130,0 339,7 240,0 1,0 22,9 169,0
4. Masic flow (kg/h) 60.000 60.000 256.360 22.431 105.603 83.172 226.449 150.757 394.978 324.000 1.290 30.955 228.150
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** ** ** **
9. N % wt 0,27 0,27 2,41 2,41 2,41 2,41 2,47 2,41 2,49 6,53 6,53 6,53 6,53
10. P2O5 Av. % wt 0,08 0,08 9,91 9,91 9,91 9,91 9,74 9,91 10,09 18,50 18,50 18,50 18,50
11. H2SO4 free % wt 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00
12. K2O % wt 0,08 0,08 0,82 0,82 0,82 0,82 0,81 0,82 0,85 1,07 1,07 1,07 1,07
13. H2O % wt 98,52 98,52 78,09 78,09 78,09 78,09 78,32 78,09 77,58 44,67 44,67 44,67 44,67
14. Solids % wt 1 max. 1 max. 6 max. 6 max. 6 max. 6 max. 6 max. 6 max. 6 max. 10 max. 10 max. 10 max. 10 max.
15. Temperature C 55,5 45,0 61 61 61 61 73,5 61 54,5 84 84 84 84
16. Pressure (g) 3 3 3 3 3 3 Grav. 3 Grav. 4 4 4 4
Kg/cm2 (wc m.m)
17. Density 990 992 1160 1160 1160 1160 1158 1160 1163 1350 1350 1350 1350
Kg/m3 at T C
pH= 5.5 pH= 5.5 N/P=0,90 N/P=0,90 N/P=0,90 N/P=0,90 N/P=0,95 N/P=0,90 N/P=0,92 N/P=0,46 N/P=0,46 N/P=0,46 N/P=0,46
18. Remarks
T max. T max. T max. T max. T max. T max. T max. T max. T max. T max. T max. T max. T max.
60C 60C 75C 75C 75C 75C 85C 75C 75C 100C 100C 100C 100C
Sheet 9 of 9
Stream number 666 670 680 681 682 690 691 692 695 700 710
Washing Phosacid Total flow Washing Washing Washing Washing Liq.Transfer Liquid Discharge Discharge
Denomination liquor to liquor to of 02-P-302 liquor to liquor to liquor to liquor to from Dust discharge PR slurry PN slurry
Pre-Scrub. P. Reactor A/B Gran. Scr. Dryer Scr. Dust Scr. Dust Scr. Scrub. to from Dust "A" or "B" to to
Duct "A" or "B" Ventury Ventury Ventury Arm Scr.Vessel Scrubber Granulator Granulator
1. Flow units m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h m3/h t/h m3/h
2. Design flow 50 30 350 125 225 102 146 30 248 40 40
3. Normal flow 47,1 5,4 336,0 120,0 216,0 98,0 120,8 19,4 217,4 7,9 24,55
4. Masic flow (kg/h) 63.605 8.463 389.760 139.200 250.560 100.940 124.424 19.960 224.486 7.924 39.288
5. Dry air (kg/h) ** ** ** ** ** ** ** ** ** ** **
6. Rel. Humidity (%) ** ** ** ** ** ** ** ** ** ** **
7. NH3 in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** **
8. Dust in air (mg/Am3) ** ** ** ** ** ** ** ** ** ** **
9. N % wt 6,53 0,99 2,41 2,41 2,41 0,51 0,51 0,51 0,56 14,86 15,50
10. P2O5 Av. % wt 18,50 43,51 9,91 9,91 9,91 2,08 2,08 2,08 2,12 46,67 14,58
11. H2SO4 free % wt 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00
12. K2O % wt 1,07 0,16 0,82 0,82 0,82 0,36 0,36 0,36 0,39 0,17 0,84
13. H2O % wt 44,67 26,47 78,09 78,09 78,09 94,69 94,69 94,69 94,45 4,71 11,88
14. Solids % wt 10 max. 10 max. 6 max. 6 max. 6 max. 4 max. 4 max. 4 max. 4 max. 95,3 88,1
15. Temperature C 84 44 61 61 61 35 35 35 35 135-140 120-125
16. Pressure (g) 4 3-7 3 3 3 3 3 3 Grav 2 2
Kg/cm2 (wc m.m)
17. Density 1350 1565 1160 1160 1160 1030 1030 1030 1033 1550 1600
Kg/m3 at T C
N/P=0,46 N/P=0,03 N/P=0,90 N/P=0,90 N/P=0,90 N/P=0,65 N/P=0,65 N/P=0,65 N/P=0,71 N/P = 1,45 N/P = 0,86
18. Remarks Flow to Tmax 155C Tmax 135C
T max. one PR Two pumps T max. T max. T max. T max. T max. T max. Flow from
100C "A" or "B" in service 75C 75C 45C 45C 45C 45C one PR
CHAPTER 9- DIAGRAMS
9.1.- PROCESS FLOW DIAGRAMS

9.2.- PIPING AND INSTRUMENTATION DIAGRAMS

9.3.- INTERLOCK DIAGRAMS

ANNEX 1.- TEST PROCEDURES

ANNEX 2.- AOAC TEST PROCEDURES

ANNEX 3.- PHYSICAL PROPERTIES OF FERTILIZER

Operating Manual NPK Phonska II

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OPERATING MANUAL Plant: R&F OPERATION PF-1 PLANT

CHAPTER 2 - PLANT DESCRIPTION

CHAPTER 3 - PREPARATION OF THE PLANT

CHAPTER 4 - GENERAL CONTROLS OF THE PLANT

CHAPTER 5 - PLANT SAFETY

CHAPTER 6 - DAP and NPK MANUFACTURE

CHAPTER 7 - PHYSICAL AND CHEMICAL DATA

CHAPTER 8 - MASS AND ENERGY BALANCES

1.2 BASIC CHARACTERISTICS OF THE PROCESS

1.3 DESIGN BASIS

1.3.1 Climatic conditions

1.3.2 Raw material specification (At battery limit)

1.3.3 Utilities specification

1.3.4 Plant product specification (Main products)

1.3.5 Production capacity

1.3.6 Plant effluents

1.3.7 Raw materials & utilities consumption (per Ton of product)

1.3.8 Input/output table at battery limit

1.2 BASIC CHARACTERISTICS OF THE PROCESS

In all cases the remaining ammonia is introduced through an ammonisation

1.3 DESIGN BASIS

1.3.2 Raw material specification (At battery limit)

P2O5 48 -50% minimum

H2SO4 content 98 % typical

Nitrogen 46% minimum

K2O 60% min.

Type Sand, clay

1.3.3 Utilities specification

Low pressure Saturated, 7 kg/cm2, for flushing

b) Process / service water

1.3.4 Plant product specification (Main products)

NPK 23.10.10 15.15.15 DAP MAP OTHER NPK

1.3.5 Production capacity

Product Dry Min Throughput (t/h) Production (t/h)

Other NPKs 12.5-20 212-314 241-374 318-375 1140-1615 1187.5-2000

1.3.6 Plant effluents

Gaseous Exhaust Stack Vent Analysis

1.3.7 Raw materials & utilities consumption (per Ton of product)

The following consumptions of raw materials are guaranteed in kg by ton of product.

Items 23-10-10 23-10-10 15-15-15 15-15-15 (H2SO4) DAP (alt. 1)

Items DAP (alt.2) 20-10-10 MAP 13-13-17-2

1.3.8 Input/output table at battery limit

Pressure Temp. C Quantity (3)

Sulphuric acid 4 kg/cm 2 Ambient 30 MT/h (4) 60 MT/h (4)

Liquid ammonia (1) 12 kg/cm 2 -33 15 MT/h 30 MT/h

Filler Grav. Ambient 15 T/h 30 T/h

Urea Grav. Ambient 30 T/h 60 T/h

Potash Grav. Ambient 30 T/h 60 T/h

Ammonium sulphate Grav. Ambient 35 T/h 70 T/h

Kieserite Grav. Ambient 10 T/h 20 T/h

Defoamer (barrels) Ambient 0.2 m 3/h 0.4 m 3/h

Process water 3 kg/cm 2 Ambient 25 m 3/h 50 m 3/h

MP Steam (sat) 7 kg/cm 2 (2) 164 2500 kg/h 4000 kg/h

Fuel Oil / PG Ambient 150-800 kg/h1200 kg/h

CHAPTER 2.- PLANT DESCRIPTION

2.1 GENERAL DESCRIPTION OF THE UNIT

2.2 MAIN CHARACTERISTICS OF THE PLANT DESIGN AND OPERATION

2.3 INTERLOCKING SYSTEM

2.1 GENERAL DESCRIPTION OF THE UNIT

Product Production (t/h)

15.15.15 (H2SO4) 1320 1375

2.1.2 Description of the equipment

Reference is made to the process flow diagrams numbers: P-05-12-300-001 and P-