Davidbrooker1 Improving Granulation Techniques PDF

Thesis David Brooker
E1445
Thesis Design
Improving Granulation Techniques

Of 'N-Gold' Fertilizer
Department of Chemical Engineering
David Brooker
Supervisor:
Jim Litster
Tony Brown
15/10/99
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ABSTRACT
An investigation was undertaken into the granulation of 'N-Gold'; a urea based fertiliser
produced at Incitec's Gibson Island granulation facility. Uncharacteristically high recycle
ratios in the order of 7:1 are observed in the production of 'N-Gold' leading to high
production costs. The study was aimed at identifying methods that can be used to reduce
the amount of fertiliser recycled in the circuit. Following a sampling audit of the process,
a range of methods were used to investigate the granulation of 'N-Gold' including size
analysis, image analysis, x-ray diffraction and a computer simulation.
The investigation found that both random and preferential coalescence mechanisms
contribute to the granulation process. As the moisture content in the system increases,
the range of the granulator outlet size distribution spreads due to a greater contribution by
the preferential coalescence mechanism. Within the granulator, a large proportion of the
fine material below 225 microns is successfully agglomerated. Much of this fine material
is produced during the crushing and screening stages of the circuit aiding in the size
enlargement process.
Image analysis indicates the formation of four different particle types; large agglomerates
in the particle size range; deformagle agglomerates attached to non-deformable crystals;
agglomerates of non-deformable particles; large spherical agglomerates outside the
product size range. In addition there are many particles that pass through the granulator
without undergoing any size enlargement. The majority of these particles are in the
intermediate size range of 0.225mm to 1mm.
The x-ray diffraction results indicate that components other than urea are present in 'N-
Gold'. It is likely that this is due to the binder content of the system. Further study is
required to identify the composition of the impurities.
The results of the sampling process were used to model the 'N-Gold' process on the
Nimbus simulation package developed by Jang (1996). A combination of sampling and
modeling limitations reduced the effectiveness of the model validation on 'N-Gold'
granulation. The results provide a solid foundation for future modeling of the process.
It has been concluded that the non-deformable particles in the size range of 0.225 mm to
1mm in the urea feed are a major contributing factor to the large recycle ratios. Grinding
the urea fines feed before it is granulated would greatly improve the granulation
efficiency. In addition effective control of the moisture content in the system will ensure
that granulation proceeds by both random and preferential coalescence mechanisms.
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Table of Contents
Chapter 1
1.0 Introduction 6
1.1 Fertiliser Granulation 6
1.2 Thesis Objectives 7
Chapter 2
2.0 Literature Review 8
2.1 Granulation Mechanisms of Fertilisers 8
2.2 Effects of Binder Content and Viscosity on Granulation 10
2.3 Effect of Initial Size Distribution 11
2.4 Effect of Circuit Performance on Granulation 11
2.5 Granulation Modeling and Simulation 12
2.6 'N-Gold' Analysis 13
2.7 Scope of Work 13
Chapter 3
3.0 Plan of Study 14
3.1 Data Collection 14
3.2 Quantity of Samples 14
3.3 Sample Analysis 15
3.4 Model Fitting and Simulation 15
3.3.1 Model Development 15
3.3.2 Model Fitting 15
Chapter 4
4.0 Experimental Procedure 16
4.1 Sampling 16
4.1.1 Sampling Procedures 16
4.2 Size Analysis 17
4.2.1 Particle Size Analysis Procedure 18
4.3 Moisture Content Analysis 19
4.4 Image Analysis 19
4.4.1 Stereomicroscope 19
4.4.2 Camera 19
4.4.3 Scanning Electron Microscope 20
4.5 X-Ray Diffraction 20
Chapter 5
5.0 Results / Discussion
5.1 Analysis of Data Collection Reliability 21
5.1.1 Sampling Errors 21
5.1.2 Precision of Sampling 21
5.1.3 Sieving Enduced Errors 22
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5.2 Results of 'N-Gold' Data Collection 23

5.3 Morphology of Particles 26
5.3.1 Scanning Electron Microscope Analysis 32
5.4 X-Ray Diffraction Analysis 32
5.5 Recycle Ratio Reduction Techniques 36
5.6 Conclusion 36
Chapter 6
6.0 Granulation Simulation
6.1 Model Development 37
6.2 Model Fitting - Granulation Drum 38
6.2.1 Size Distribution 38
6.2.2 Physical Constants 39
6.2.3 Empirical Constants 40
6.3 Model Fitting for Granulator 42
6.3.1 Initial Conditions 42
6.3.2 Model Fitting 42
6.4 Conclusion 46
Chapter 7
7.0 Conclusion 47
Chapter 8
8.0 Nomenclature 48
Chapter 9
9.0 References 49
Appendix 1 Physical Properties of Fertilisers 51
Appendix 2 Granulation Simulation 52
Appendix 3 Sampling Error 53
Appendix 4 Precision of Sampling 54
Appendix 5 Raw Data 55
Appendix 6 Nimbus Code 51
Appendix 7 Granulator Initial Conditions 66
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List of Figures
Figure 1 - 'N-Gold' Granulation Circuit 6
Figure 2 - Major Granulation Mechanisms 8
Figure 3 - Pendular, Funicular and Capillary States of the Mobile Liquid Phase 10
Figure 4 - Variation of Recycle Ratio with Solution Phase Ratio (Adetayo 1995) 11
Figure 5 - Sampling Points 16
Figure 6 - Granulator Exit Sampler and General Purpose Sampling Device 17
Figure 7 - Sieve Shaker 18
Figure 8 - Camera used for Image Analysis 19
Figure 9 - Precision of Sampling Results 21
Figure 10 - Effect of Sieving Process on Particle Size Distribution 22
Figure 11 - Size Distribution of Urea Fines 24
Figure 12 - Comparison of the U-Fines Feed to the Granulator Exit Flowrate 24
Figure 13 - Change in Size Distribution over the Granulator, Run 1 25
Figure 18 - Effect of Moisture Content on Range of Particle Size Distribution 27
Figure 19 - Effect of Binder Flowrate and Steam Pressure on the Particle Size Range 28
Figure 20 - Comparison of Size Distribution for Granulator and Drier Exit, Run 1 28
Figure 21 - Morphology of U-Fines 30
Figure 22 - Morphology at Granulator Exit 30
Figure 23 - Effect of Particle Deformation on Bond Strength (Adetayo, 1993) 31
Figure 24 - Electron Microscope Image 52x Magnification 33
Figure 25 - Electron Microscope Image 1033x Magnification 34
Figure 26 - X-Ray Diffraction Results 35
Figure 27 - Granulation Circuit of Di-Ammonium Phosphate (Jang, 1996) 37
Figure 28 - Granulation Circuit for 'N-Gold' Process 38
Figure 29 - Effect of Size Independent Kernel on Granulation 40
Figure 30 - Effect of Size Dependent Kernel on Granulation 41
Figure 31 - Effect of Changing β (u , v ) (Adetayo) 41
Figure 32 - Comparison of Sampling to Simulation Results, Run 1 41
Figure 37 - Effect of Moisture Content on Size Distribution 45
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1.0 INTRODUCTION
1.1 Fertilizer Granulation
This thesis investigates problems associated with the granulation process during the
production of 'N-Gold'. 'N-Gold' is a urea-based fertilizer produced by granulating urea
fines (u-fines) at Incitec's granulation plant on Gibson Island. Granulation is the general
term relating to the gathering of smaller particles into a larger mass. There are many
methods of granulation including compression, extrusion, agglomeration, globulation,
nodulization and sintering. The method of granulation used depends on the application
and type of particle to be granulated. The fertilizer industry is one of many industries
that use agglomeration to increase particle size. Granulated fertilizer has excellent
storage, handling and transportation properties and allows the controlled release of
nutrients.
'N-Gold' is a relatively new product that is not produced elsewhere in the world. As a
result little information exists about its granulation properties. Figure 1 shows the
granulation circuit at Incitec. A particulate phase is mixed with a liquid binder in the
granulation drum, which adds a shearing force to facilitate size enlargement. The
granulated material is then dried in a co-current rotary drier. The fertilizer then passes
through a set of oversize and undersize screens to separate out the product. The
oversized material is then crushed and recycled with the undersized stream.
Liquid Feed
Granulation Dry Granule
Powder Feed Rotary Drier
Drum
Product
Screen
Undersize
Recycle Oversize
Recycle
Crusher
Figure 1: 'N-Gold' Granulation Circuit
The granulation circuit poses two main problems:

1. A relatively small amount of particles are in the desired size range. As a result large
recycle streams are necessary, often exceeding of 7:1.
2. Problems of surging, drifting mass flow rates and large size distributions along with
large time constants mean that the process is difficult to optimize and control.
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Compared with the other fertilizers produced at Incitec, the 'N-Gold' production process
exhibits unusually large recycle ratios with low product rates. This leads to an increase
in cost due to low production rates.
1.2 Thesis Objectives

The aim of this thesis is to analyse the 'N-Gold' production process and identify methods
of improving the granulation efficiency of 'N-Gold', allowing a reduction of the recycle
ratio and improved circuit control. This will result in increased profit for Incitec. To
achieve this, the following objectives have been addressed:
v Perform a plant audit on the 'N-Gold' granulation process
v Analyse the data using a range of particle characterization techniques
v Simulate the 'N-Gold' granulation circuit using existing modeling facilities
v Identify methods to reduce the recycle ratio and improve circuit control.
This thesis continues on from the work of G. Davis in 1996 who investigated the
granulation of 'N-Gold' and an ammonium sulfate based fertilizer.
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2.0 LITERATURE REVIEW

2.1 Granulation Mechanisms of Fertilizers
A range of mechanisms for granule growth has been discussed in literature. These
include the nucleation, coalescence and layering (Snow, 1997). Figure 2 outlines these
main size enlargement processes.
Coalescence
Nucleation
Layering
Figure 2: Major Granulation Mechanisms
Experimental observations of granulation processes indicate that the mechanisms of size

enlargement are often unique to a given class of materials (Adetayo and Ennis, 1997).
This has also found to be true between different types of fertilizers. Fertilizers can be set
aside from other granulated materials for a number of reasons.
1. Fertilizer granules are hard and cannot easily be deformed. This reduces the ability of
the particles to dissipate breakup forces during granulation resulting in lower growth
rates (Adetayo and Ennis, 1997).
2. The second factor effecting the granulation of fertilizers is their solubility.

Sherrignton (1968) found that the differing solubilities of particles partly explained
the variation in granulation properties of different fertilizers. Therefore the chemical
composition of the particle has a significant effect on the granulation process.
Appendix 1 summarizes the physical characteristics of a range of fertilizer compounds. It

can be seen that 'N-Gold' has significantly higher solubility then other fertilizers. This
difference partly explains the granulation differences between 'N-Gold' and other
fertilizers produced at Incitec.
Adetayo et al. (1993) proposed that the main mechanism of granulation for fertilizers is
coalescence with a minor effect resulting from layering. Ennis et al. (1991) proposes a
two stage coalescence mechanism:
1. The first stage of granulation is a fast and short-lived process. Size enlargement
proceeds by random coalescence where nearly all collisions result in new
agglomerates. Therefore a successful coalescence is independent of the particle size
and collision velocity. This process has the effect of narrowing the particle size
distribution. The extent of granulation by the first stage of coalescence is determined
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by the point at which the resultant Stokes number is equal to the critical stokes
number. The resultant Stokes number for rotary drum granulation is
8ρ g r ω R
given by: St v =
9µ
Where
ρ g = Granule density, g/cm3
r = Effective granule size, m
ω = Drum speed, s-1
R = Radius of granulation drum, m
µ = Binder Viscosity, P
At low moisture contents this is the only mechanism.
2. When sufficient moisture is provided a second stage of granulation occurs called

preferential coalescence. Under preferential coalescence not all collisions are
successful. Granulation is influenced by factors such as the material type, solution
viscosity, surface tension, particle deformability and liquid content. A successful
collision relies on granule compaction to squeeze binder to the granule surface.
This two-stage growth mechanism was validated by Adetayo et al (1995) for granulation
of di-ammonium phosphate fertilizer. Zhang (1996) has used the mechanism in the
development of the dynamic model of the fertilizer granulation circuit.
For optimum circuit performance the process should be controlled between the two stages
of granulation. This has the effect of removing all the fines from the recycle without
broadening the particle size distribution (Adetayo, 1993).
An alternative approach to modeling fertilizer granulation mechanisms was developed by

Bathala et al. (1998). They proposed that the granulation process is governed by layering
mechanisms. Under this process size enlargement occurs by layers of small particles
forming on existing particles. The growth rate is assumed to be inversely proportional to
the existing particle size and the size to which it grows.
Iverson and Litster (1997) proposed the most recent development in granulation
mechanisms. They constructed of a regime map to describe the granule growth as a
function of the particle deformability and the pore saturation. The proposed mechanism
is based on two broad regimes:
1. Steady Growth. This regime is for a highly deformable system capable of
withstanding the separating forces in the granulator.
2. Induction. This occurs for systems with strong, non-deformable and slow
consolidating particles.
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The regime map is based on properties of the powder binder system. It therefore has the
potential to be used for the prediction of the granulation behaviour without the need for
granulation experiments.
2.2 Effects of Binder Content and Viscosity on Granulation
For any granule agglomeration or growth to occur, a minimum amount of binder must be
added to the process. The binder facilitates coalescence through the formation of a
mobile liquid bridge that generates interfacial forces and capillary suction between
particles. This mobile liquid phase can form in three states, pendular, funicular and
capillary. These three states are indicated by Figure 3. In the pendular state the liquid is
held in discrete lens shaped rings at the point of contact between particles. An increase
of binder leads to the funicular state where a continuous fluid network with interspersed
air is generated. At the point of complete saturation the capillary state is formed. In this
state all the pore spaces are filled (Snow et al, 1997).
Pendular Funicular Capillary
Figure 3: Pendular, funicular and capillary states of the mobile liquid phase.
The amount of binder required to reach each of these states is related to the powder
porosity, particle surface area and binder-powder wetting characteristics. In addition to
theses properties the factors effecting agglomerate formation include:
v Initial binder mixing distribution.
v Time required for the binder to spread and penetrate pores. (ie. Binder wetting,
spreading and adsorption characteristics)
v Time taken for the binder to strengthen. This is effected by the evaporation of
solvent, reactive transformations, cooling and other solidification mechanisms.
The extent of granulation is a function of binder content present during granulation. This
is termed the liquid phase ratio. The mean granule diameter increases with the amount of
free liquid available for coalescence. As the liquid phase ratio increases both the rate and
extent of granulation increases (Adetayo and Ennis, 1997). Adetayo et al. (1995) shows
that as the liquid phase ratio increases the recycle ratio of the granulation circuit goes
through a minimum. This minimum recycle ratio is reached when the majority of
particles leaving the granulator are in the desired product size range. Figure 4 shows a
plot of the recycle ratio as a function of solution phase ratio. The plot was developed
using the results of a steady state fertilizer simulation developed by Adetayo et al. (1995).
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Figure 4: Variation of recycle ratio with solution phase ratio. (Adetayo, 1995)
2.3 Effect of Initial Size Distribution
Granulation experiments performed by Adetayo et al (1991) showed that the inlet size
distribution fed into the granulator has a significant effect on the resultant particle size
distribution of the granulated material. It was found that as the amount of fines in the
feed increased the median particle diameter passes through a maximum for a given
moisture content. This indicates that there is an optimum feed rate at which the urea
fines can be added to maximize the extent of granulation.
The effect of removing the coarse particles from the feed was also investigated. It was
found that the amount of coarse particles in the feed strongly effects the particle size
distribution.
2.4 Effect of Circuit Performance on Granulation
In addition to the granulator, the granulation circuit also contains a drier, crusher and
screen. The effect of these units has a significant effect on the performance of the circuit.
Adetayo et al. (1995) investigated the effect varying the granulation circuit parameters on
the performance of the steady state circuit. They found that increased crusher efficiency
will reduce the recycle ratio and improve circuit control. The crusher has the effect of
changing the particle size distribution fed to the granulator. An efficient crusher will
narrow the particle size distribution in the feed by reducing the number of coarse
particles. The steady state results agree with the experimental observations of Adetayo et
al (1993) who found that the amount of coarse particles had a significant effect on the
particle size distribution being fed into the granulator.
The steady state analysis carried out by Adetayo et al. (1995) also showed that an
increase in the screen performance had a significant effect on the reduction of the recycle
ratio. The screen however had no effect on the allowable operating region and therefore,
did not effect the circuit stability.
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2.5 Granulation Modeling and Simulation
In the modeling of granulation process the particle size distribution is the most important
quantity. The change of the size distribution with time and position in the granulator is
followed using a population balance. The general form of the population balance is given
by:
∂n(v, t ) Qin Q ∂(G * − A*)n(v.t )

= nin (v) − ex nex (v) − + Bnuc(v)
∂t V V ∂v
∫ β (u, v − u, t )n(u, t )n(v − u, t )du

1 y
+
2N t 0
∞
∫ β (u, v − u, t )n(u, t )n(v − u, t )du
1
− (Snow et al., 1997)
Nt 0
Where:
V = Volume of granulator
Q = Inlet and exit flowrates from granulator.
G (v ) = Layering rate
A(v ) = Attrition rate
Bnuc (v) = Nucleation rate
β (u , v, t ) = Coalescence kernel
N t = Total number of particles per unit volume
In general this population balance cannot be solved by analytical methods. It is therefore

necessary to solve it using numerical techniques. Hounslow (1988) proposed a method to
discretize the size domain such that vi + 1 / vi = 2 . This method is widely used in
population balance modeling.
An important factor in the fitting of the population balance to the granulation process is
the coalescence kernel ( β (u , v, t ) ). The kernel dictates the birth and death rates during
granulation. The development of the correct coalescence kernel requires an
understanding of the granulation mechanisms and will therefore vary depending on the
application.
Recent research has identified improvements in the modeling of granulation of fertilizers.

In 1995 Adetayo et al. developed a simulator of a steady state fertilizer granulation
circuit. The population balance used the two-stage coalescence kernel developed by
Ennis et al. (1991). This simulation was validated by a series of experiments on the
granulation of a di-ammonium phosphate fertilizer. Zhang (1996) adapted this simulation
to develop a dynamic model of a fertilizer granulation circuit.
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An alternative approach to modeling a dynamic fertilizer granulation process was

developed by Bathala et al. (1998) using a model based on layering mechanisms (see
section 2.1). This model was validated on a nitrogen-potassium fertilizer system.
2.6 'N-Gold' Analysis
Limited research has been carried out on the granulation performance of 'N-Gold' to date.
Davis (1996) carried out an investigation into the differences between 'N-Gold' and
ammonium sulfate. This investigation concentrated on sampling from the granulation
circuit at Incitec. Davis found that 'N-Gold' exhibits similar granulation properties to
other commercial fertilizers. The investigations also found that 'N-Gold' has a minimum
obtainable recycle ratio of 5.6:1. Davis results agreed with Adetayo et al. (1995). He
found that the minimum recycle ratio was reached as the moisture content is increased.
Davis (1996) concluded that the granulation properties of 'N-Gold' are sufficiently similar
to other fertilisers to allow the adaptation of existing simulation packages to model 'N-
Gold' granulation.
2.7 Scope of Work
Work in the area of fertilizer granulation has increased the understanding of the
underlying mechanisms. The aim of this thesis is to identify why limited granulation of
'N-Gold' occurs when compared with the other fertilizers produced at Incitec. Davis
(1996) investigated the granulation of 'N-Gold'. His research was however limited to the
analysis of the particle size distribution. This thesis will continue from previous work by
performing further analysis of 'N-Gold'. In addition the data collected on the processing
of 'N-Gold' will be used to model the granulation of 'N-Gold'. Significant research has
been carried out in the modeling of granulation processes. The existing fertilizer
granulation simulator developed by Zhang (1996) will be used. Zhang's model suits the
purpose as it has been validated for fertilizer granulation and it is a dynamic model. A
dynamic model is important in the analysis of circuit control.
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3.0 PLAN OF STUDY

3.1 Data Collection
A plant audit was carried out over the 'N-Gold' granulation facility. The audit was
performed over a period of three days in March 1999. Additional sampling was
proposed for the period June-August. Due to a changed plant schedule this sampling
could not proceed. The aim of the audit was to identify the granulation characteristics of
'N-Gold' under normal operating conditions. Table 1 outlines the data collected from the
'N-Gold' granulation circuit.
Table 1: Data Requirements

Stream Particle Size Moisture Temperature Flowrate
Distribution Content
Recycle to Granulator X X X X
(s) (s) (s) (p)
Fertilizer flow into X X X X
Granulator (s) (s) (s) (p)
Binder flow into X
Granulator (p)
Steam flow into X
Granulator (m)
Fertilizer flow out of X X X X
Granulator (s) (s) (s) (p)
Fertilizer Flow out of X X X
Drier (s) (s) (s)
Air Flow into Drier X
(p)
Air Flow out of Drier X
(p)
s - Data taken from plant sample
p - Data taken from plant control panel
m - Data taken from plant reading
The temperature of the fertilizer throughout the circuit was measured using an infra red
non-contact temperature sensor. The accuracy of the measurement is ± 0.1oC.
3.2 Quantity of Samples
'N-Gold' is only produced several times each year. Each production run of 'N-Gold'
continues for several weeks. To maximize the value of the audit, data is required from
the 'N-Gold' process under a variety of operating conditions. There was no possibility
however, of setting the operating conditions under which the plant operates. A total of
five sets of samples were taken.
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3.2 Sample Analysis
The following analysis has been performed on the samples:

v Size Analysis. Sieving was used to analyse the size distribution.
v Moisture Content.
v Image Analysis. Image analysis allowed visual examination of the smaller particles
within the sample.
v X-Ray Diffraction. X-ray diffraction was used to analyze the chemical make-up of
the particles and check for the presence of binder.
3.3 Model Fitting and Simulation
The dynamic simulator developed by Zhang (1996) was used in the analysis of the 'N-
Gold' process. The characteristics of the simulator are shown in appendix 2.
3.3.1 Model Development
The current simulator models the production of di-ammonium phosphate. This model
was adapted to suit the 'N-Gold' process. The changes that were made include:
1. The addition of a mixing unit to mix the urea fines and the recycled material.
2. The elimination of the unsuitable mechanisms from the granulator.
3.3.2 Model Fitting
The data collected from the plant audit was used to fit the simulator to the 'N-Gold'
process. Three main factors needed to be adjusted:
1. Specifying initial conditions.
2. Adjusting physical constants.
3. Identifying appropriate empirical constants.
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4.0 EXPERIMENTAL PROCEDURE

The following section outlines the procedures involved in carrying out plant sampling
and the analysis of the results.
4.1 Sampling
Sampling was concentrated around the granulation drum. The location of each of the
sampling points is outlined in figure 5.
1. Granulator Feed
2. Urea Fines Feed
3. Granulator Exit
4. Drier Exit
Liquid Feed
4
Granulation Dry Granule
Urea Fines Rotary Drier
Drum 3
2 1 Product
Screen
Undersize
Recycle Oversize
Recycle
Crusher
Figure 5: Sampling Points
4.1.1 Sampling Procedures
The quality of the samples taken for size analysis was limited by the error in the sampling
procedures. Good sampling tools and appropriate sampling techniques can minimize this
error.
There are two main sources of error in sampling of particulate solids. These are
delimitation and extraction errors. Delimitation errors arise when not all of the particles
in a stream have equal probability of being sampled. Extraction errors occur when the
probability of the particles occurring on the edge of the increment being sampled is size
dependent.
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In order to take a representative sample the following rules should be followed:
v A powder should always be sampled while in motion.

v The whole of the stream of powder should be sampled for many short increments of
time in preference of part of the stream being taken for the whole time.
It is therefore necessary to design the correct sampling equipment to obtain a

representative sample. The following criteria should be followed in the design of a
sampler (Snow et al, 1997):
v Cutter width should be at least 3 times the diameter of the falling stream
v Cutter length should be at least 10mm or three times greater then the largest particle
v Sampler should not become more than half full.
Even when correct techniques eliminate bias, sampling variance will still arise. This
variance is a result of short and long term fluctuations in the process being sampled. The
long-term fluctuations are a result of effects generated by the process including
fluctuations in the flow rate. Short term fluctuations result from variability within
particles.
Figure 6 shows the sampling tools used in the plant audit. The sizes of the tools are
limited by the size of the access points in the granulator circuit.
250
10
250
0
10
0
100
100
B
A
Figure 6: A - Granulator exit sampler; B - General purpose sampling device
4.2 Size Analysis
Sieving was used to analyze the particle size distribution of the fertilizer samples. A 2
sieve series between 0.053 and 11.2 mm aperture was used in the analysis. In this series
the area of successive screens has a constant ratio of 2. A 2 sieve series has been
chosen as it provides acceptable loading on each of the screens.
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The factors effecting the accuracy of sieving are:
v Sieving time
v Characteristics of the particle
v Particle load on the sieve
v Method of shaking the sieve
v Geometry of the sieve surface
v Angle of presentation of the particle to the aperture.
The amount of separation achieved is a function of the sieving time. By maintaining a

constant sieving time, constant sieving equipment and approximately constant sample
size the variance in the analysis of samples can be minimized.
A Retsch AS200 Analytical Sieve Shaker has been used in the analysis of the particle
size. The amplitude of the vibration was set to 50. This corresponds to a vibration height
of approximately 1.6mm. The sieve shake is shown in figure 7.
Figure 7: Sieve Shaker
4.2.1Particle Size Analysis Procedure
1. The original sample size taken from the granulator circuit is in the order of 1 kg. To
keep an acceptable particle load on the sieve the sample size needed to be reduced to
approximately 200-300g. The sample will therefore be split twice using a chute
splitter. The chute splitter will introduce a variance of approximately 3.4% (Snow et
al, 1997).
2. The number of sieves used in the analysis was too large to be held by the sieve
shaker, therefore the fertilizer was screened in two stages. The first stage involved
passing the material through sieves with an aperture ranging from 11.2mm→ 0.71mm.
The sieving time for this stage is 10 minutes.
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3. The second stage of the sieving involves passing the undersized material from the
first pass through sieves with an aperture ranging from 0.5mm→ 0.053. The sieving
time for this stage is 10 minutes.
4.3 Moisture Content Analysis
The moisture content of 'N Gold' was found by drying the fertilizer in a drying oven. 'N-
Gold' begins to melt at 80 to 90 oC depending on the level of impurities. The drying
process is outlined below:
1. Initial weight of sample recorded.
2. Sample dried in oven at 70 -75oC for 24 hours.
3. Final Mass of Sample recorded.
4.4 Image Analysis
Image analysis allows the physical examination the particles throughout the granulation
circuit. Three methods were used to capture the images of the particles.
4.4.1 Stereomicroscope
An Olympus CH-I stereomicroscope with an image capture facility was used to perform
thee image analysis on the particles of size 250 microns and below. The eyepiece
magnification was 10x with a set of objective lenses ranging from 5-85x magnification.
4.4.2 Camera
A single lens reflex camera was used to capture the image of particles in the size range of
710 microns and above. A Pentax single ten was set up with a 115mm telephoto lens, a
2x doubler and a standard 50mm lens mounted in the reverse direction on the front of the
telephoto lens. This configuration gives a 22x magnification. An electronic flash was
used to side light the particle with a mirror positioned opposite the flash to act as a back
fill light source. The flash synchronization speed was set at 1/60 second. The aperture
size was set at f16 for the 50mm lens and f11 for the telephoto. The configuration is
shown in figure 8.
Figure 8: Camera used for Image Analysis
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4.4.3 Electron Scanning Microscope
The Philips XL30 scanning electron microscope was used to take detailed images of the
fertilizer surface. An accelerating voltage of 10kV was used. The samples were carbon
coated to minimise charging. To remove any absorbed water within the particles, they
were first evacuated overnight. This process may have effected the morphology of the
particles.
4.5 X-Ray Diffraction
X-Ray diffraction was used to collect data on the chemical makeup of the 'N-Gold'
particles. A Siemans D5000 goniometer with Cu Kα radiation was used in the analysis.
Search / match software was used to identify the peaks in the output.
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5.0 Results / Discussion
5.1 Analysis of Data Collection Reliability
5.1.1 Sampling Errors
Errors are induced into the results due to sampling of the fertiliser in the granulation
circuit. An estimate of the short term errors induced into the process can be made using
Gy's theory (Smith and James, 1981)
1 1
σ 2 = ρx(100 − x)  − lα v hd 95
3
 s
M M 
Where
ρ = Density of particle l = Degree of liberation
x = Property being measured (mass fraction) α v = Volume shape factor
M s = Mass of sample h = Spread of size distribution
M = Mass from which sample is taken d 953 = 95% passing size of distribution
The sampling error for the samples taken at the granulator outlet has been calculated in
appendix 3. The maximum sampling error was found to be 15.53%.
5.1.2 Precision of Sampling

In order to test the precision of the sampling techniques a series of four samples were
taken in quick succession from the entrance to the granulator. A plot of the mass fraction
of the size distribution for each sample is shown in figure 9.
0.35
Test A
0.3 Test B
Test C
0.25 Test D
Mass Fraction
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
Figure 9: Precision of Sampling Results
22
The plot shows that there is a small variation in the size distribution of the four samples.
It can be seen that test sample B has twice the proportion of fines when compared with
the other samples. This variation can be explained by changes in the particle size
distribution in the granulator entrance over the sampling time and by limitations
associated with taking a representative sample from the granulator feed.
To quantitatively assess the variance in the sample, the standard error at each size interval
was calculated. The standard deviation at each size interval is given by:
Σ( yi − y ) 2
σ =
2
n− 1
where:
y =Average mass at given size interval
yi = Mass at given size interval
n = Number of size intervals.
Appendix 4 shows the calculation of the standard deviation and standard error at each
size interval. The average error over each of the 17 size intervals was found to be 1.5%.
The greatest error of 4.4% was found to occur in the size range of 1.4 to 2mm. The small
errors indicate that there is only a small difference in the size distribution for the four
samples. This is insignificant when compared to the sampling errors outlined in section
5.1.1. It can therefore be concluded that the sampling procedures produce precise results.
5.1.3 Sieving Induced Errors

The effect of the sieving process on the size distribution of the particles has been
investigated by repeatedly sieving the same sample. Figure 10 shows a plot of the
particle size distribution after sieving for 5, 7,10 and 15 minutes.
0.25
5min
7min
0.2
10min
15min
Mass Fraction
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
Figure 10: Effect of Sieving Process on Particle Sieve Distribution
23
The plot shows that there is a negligible shift in the particle size range as the sieving time
is increased. Any change in the particle size distribution is a result of fines generation
and increased separation efficiency. When the effect of the sieving process is compared
with the precision of the sampling shown in figure 8, it can be seen the sieving has an
insignificant effect on the particle size distribution.
5.2 Results of 'N-Gold' Data Collection
Table 2 outlines the 'N-Gold' operating conditions resulting from the audit of the
granulation circuit. Four sampling points were used, the feed to the system (u-fines), the
granulator entrance, the granulator exit and the drier exit. Five sets of samples were
collected. (Appendix 5 shows the raw sampling data.)
Table 2: 'N Gold' Operating Conditions

Run Liquid D50 Gran D50 Gran Gran Exit Gran Exit Steam Mass % in
Feed Entrance Exit %H2O Temperature Pressure Product Size
(L/s) (o C) Range (2-4mm)
1 0.31 0.68 1.1 0.02 46.3 21 8.5
2 0.34 0.93 1.19 0.011 51.2 34 2
3 0.22 0.95 1.28 0.0183 46.1 22 14
4 0.31 1.08 1.28 0.034 46 22 16
5 0.30 1.09 1.4 - 46.4 22 26.5
Table 3 outlines the average spread of the size distribution at each sampling point. The
spread of the distribution has been measured as D90-D10. The table shows that the particle
size distribution is broadened as the particles pass through the granulator. The drier has
little effect on the breadth of the particle size distribution.
Table 3: Spread of Particle Size Distribution

Sample D10 D90 D90-D10
U-Fines 0.132 1.87 1.74
Granulator Entrance 0.22 1.8 1.58
Granulator Exit 0.55 2.55 2.00
Drier Exit 0.25 2.21 1.96
24
Figure 11 shows the size distribution for the u-fines, the feed for the granulation circuit.
0.4
Run 1
0.35
Run 2
0.3 Run 3
Run 4
Mass Fraction
0.25 Run 5
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
Figure 11: Size Distribution Urea Fines
It can be seen that the size distribution of the urea feed varies considerably for the
different samples. A likely cause of this variation is a result of the urea fines collection
system. The feed is collected from a stockpile before being feed into the granulator. As
a result the size distribution will vary depending on where within the pile the feed is
collected. The distribution is bimodal in shape. The first peak occurs at approximately
0.3mm with the second peak at 1.5mm.
The flowrate of the u-fines is approximately 6.5 kg/s. This u-fines stream is then mixed
with the recycle stream (approximately 45 kg/s) to form the feed for the granulator.
Figure 12 shows a comparison of the normalised size distribution for the granulator feed
and the u-fines.
0.4
0.35 U Fines
Gran Ent
0.3
Mass Fraction
0.25
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
Figure 12: Comparison of the U-Fines Feed to the Granulator Entrance Flowrate
25
There is a considerably larger amount of fines in the granulator feed when compared with
the u-fines. These additional fines have two possible origins:
1. Poor granulation of the fine material in the granulator and as a result fines are
accumulating in the circuit.
2. Additional fines are being generated in the granulation circuit. The likely
source would be the crusher.
Figure 13 through to figure 17 shows the change in the particle size distribution in the
granulator for each of the five runs. All five runs show a shift in the particle size
distribution to the right indicating that size enlargement has occurred. It can be seen that
the majority of the particles in the size range 0-125 microns are consumed during
granulation. This indicates that the fines seen in the granulator entrance are a result of
fines generation within the granulator circuit, not accumulation.
0.35
Gran Ent
0.3
Gran Exit
0.25
Mass Fraction
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
Figure 13: Change in Size Distribution over the Granulator, Run 1

0.4
0.35 Gran Ent

Gran Exit
0.3
Mass Fraction
0.25
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
26
0.4
0.35 Gran Ent

Gran Exit
0.3
Mass Fraction
0.25
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)

0.3
Gran Ent
0.25 Gran Exit
Mass Fraction
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
0.4
0.35 Gran Ent

Gran Exit
0.3
Mass Fraction
0.25
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
27
Identifying the mechanisms by which granulation occurs is important in gaining an

understanding the granulation process. Adetayo et al (1993) proposed a two stage
granulation mechanism based on experiments of mono-ammonium phosphate and di-
ammonium phosphate fertilisers. In the first stage, random coalescence, nearly all
collisions are successful. The probability of coalescence equals the probability of
encountering binder during a collision. Under these conditions collisions between large
particles and fines remove fine particles from the distribution. This has the effect of
narrowing the size distribution. Inspection of the size distributions indicates that the
granulation of 'N-Gold' occurs predominately by this reaction. The fines within the
system are consumed and there is a general shift to the right in the distribution.
The second stage of granulation proposed by Adetayo et al (1993) is the size independent
kernel. Under the second stage, granulation occurs by preferential coalescence, not all
the collisions are successful. The particles may grow significantly larger then in the first
stage and as a result the size distribution is broadened. This second mechanism will only
occur at high enough moisture contents. Figure 18 shows that the size distribution of the
'N-Gold' outlet broadens with increasing moisture content. This is evidence of the effect
of preferential coalescence in the granulator. As the particle moisture content increases, a
greater proportion of the granulation occurs by preferential coalescence. For coalescence
to occur under these conditions the collision relies on the granule compaction to squeeze
additional liquid to the granule surface. The granules deform on collision increasing the
contact area of the colliding particles (Adetayo et al, 1993).
3
Range of Distribution (D90-D10)
2.5
1.5
0.5
0
0 0.5 1 1.5 2 2.5 3 3.5 4
Size (mm)
Figure 18: Effect of Moisture Content on Range of Size Distribution
There are two main variables that effect both the moisture content and level of
granulation in the system, the binder flowrate and the steam pressure. As figure 19
shows there is no correlation between either the binder flowrate or the steam pressure and
the breadth of the distribution.
28
2.8
3
Breadth of Distribution (D90-D10)

2.6
Breadth of Distribution (D90-D10)
2.5 2.4
2.2
2
2
1.5 1.8
1
1.6
1.4
0.5
1.2
0 1
0.2 0.22 0.24 0.26 0.28 0.3 0.32 0.34 0.36 0.38 20 22 24 26 28 30 32 34 36
Binder Flowrate (L/s) Steam(PSI)
A B
Figure 19: Effect of Binder Flowrate (A) and Steam Pressure (B) on the Particle Size
Range
It is difficult to draw any solid conclusions from these results. The 'N-Gold' granulation
circuit has proven to be an unstable process, producing large variations in the recycle
flowrate. As the liquid flow into the granulator is held approximately constant, the
moisture content (liquid flow / recycle flow) will also undergo large fluctuations.
Figure 20 shows that there is no net breakage or agglomeration of 'N-Gold' in the drier.
0.4
0.35 Gran Exit

Drier Exit
0.3
Mass Fraction
0.25
0.2
0.15
0.1
0.05
0
0.01 0.1 1 10 100
Size (mm)
Figure 20: Comparison of Size Distribution for Granulator and Drier Exit, Run 1
29
Size enlargement within the granulation drum is occurring by two mechanisms, random
and preferential coalescence. The amount of size enlargement is however small. Table 2
shows that for run 2 only 2% of the fertiliser out of the granulator is in the product size
range. There are two operating conditions in run 2 that standout from the other runs. The
first is that the moisture content at the granulator exit of run 2 is the lowest out of the five
runs. This leads to a narrow size distribution due to the small contribution of preferential
coalescence to size enlargement.
The second standout feature of run 2 is the high steam pressure. The pressure in run 2 is
approximately 12 psi higher then the other runs. This increased temperature did not
effect the moisture content of the system but it did have an effect on the outlet
temperature. The temperature of run 2 is 5 degrees higher then the other runs. The steam
has a significant effect on the energy input of the system. There are insufficient
variations in steam pressures within the samples taken to identify the effect of steam
pressure and temperature on granulation. 'N-Gold' however, has a melting point that is
considerably lower then other fertilizers, 80-90oC depending on the level of impurities.
Further investigation is required to identify the effect of temperature on the fertilizer
including particle deformation.
The results have shown that the fine material within the granulator, up to 250 microns, is
almost entirely consumed in the granulator. Approximately 30% of the particles are in
the size range of 250 microns to 1mm. These particles are notoriously difficult to
granulate.
5.3 Morphology of Particles

Individual particles have been removed from the bulk sample to identify the morphology
of particles within the granulation circuit. The image analysis was performed using a
single lens reflex camera (SLR) and a stereomicroscope (SM).
Section 5.2 identified that the u-fines form a bi-modal distribution. The two main particle
types that make-up this distribution are shown in figure 21.
Particle A is a prill particle. It is an undersized by-product of the prilling operations at

Incitec. The prills are hard spherical urea particles.These prill particles comprise the
majority of the particles in the 1-2mm size range. Some 710 micron prills were also
present. Particle B is a smaller urea crystal. These crystals comprise the size ranges
from 90 to 710 microns. Visual analysis of the u-fines indicates that there are no
agglomerates within the feed.
The u-fines are then mixed with the recycle where they enter the granulator. Several
particle types emerge at the granulator exit. These are shown if figure 22.
Particle A is a large 'N-Gold' particle in the product size range. It is an agglomerate of

many smaller particles.
30
Figure 22: Morphology of Particles
31
Particle B is a flat non-deformable crystal joined to a larger particle. The larger particle
has deformed upon collision with the crystal. This is further evidence of the preferential
coalescence within the system.
Particle C is two prill particles that have come together without deforming. The
probability of coalescence between two non-deformable particles is low due to the
reduced contact area. This is shown diagrammatically by Adetayo (1993) in figure 23.
Non Deformable Particles Weak Bond
Strong, increased
Deformable Particles area of contact
Figure 23: Effect of Particle Deformation on Bond Strength (Adetayo, 1993)
Due to the weak bond formation, the amount of prill - prill agglomerates out of the
granulator is low. This form of agglomerate requires the presence of binder during
collision.
On leaving the granulator, the fourth particle type, particle D, is a disc shaped
agglomerate. The workers at Incitec named these particles "Smarties". These particles
are found throughout the larger size ranges, 2mm to 8mm. Workers at Incitec reported
that the number of "smarties" increase with increasing binder flowrate. These particles
may be a result of large amounts of binder accumulating with a small amount of urea.
The final types of particles found in the system are unagglomerated prill and crystalline
particles. These particles either pass through the granulator without undergoing any size
enlargement or form weak bonds which are quickly broken again. These particles make
up the size range below 710 microns but are also present in the larger size ranges.
It is evident from the analysis of the morphology of the particles that although size
enlargement is occurring within the system, a large number of particles are passing
through the granulator unagglomerated. The majority of the particles in the U-Fines
stream are single, non-deformable particles. For the u-fines to attach to each other,
binder needs to be present at the point of collision. Alternatively the u-fines can join to
the larger agglomerates that have been recycled into the granulator. These larger
particles appear to be more deformable resulting in stronger bond formation.
32
5.3.1 Scanning Electron Microscope Analysis

A scanning electron microscope was used to identify the surface structure of the urea
prills. Figure 24 shows a prill attached to a smaller particle at a magnification of 52x.
The image displays the porous nature of the particle.
Figure 25 shows a prill at 1033x magnification. This image identifies that the prills are
composed of small crystal like grains with a size in the order of 5 microns.
5.4 X-Ray Diffraction Analysis
X-ray diffraction (XRD) has been performed on a range 'N-Gold' particles in an attempt
to identify their chemical composition. Figure 26 shows the XRD output for four particle
types:
Plot A: Fine urea crystals (90ηm) removed from the granulator exit.
Plot B: A portion of bulk urea sample from the 710 micron size range.
Plot C: An agglomerate 1mm in size.
Plot D: Material scraped from the surface of a large agglomerate.
The fine lines through each plot show the peak position of urea, the major component of
'N-Gold'.
It is clear that all plots show the characteristic urea composition. There are however
additional peaks in plots A, B and C. This indicates that material other then urea is
present in the sample. This indicates that material other then urea is present in the
samples. Attempts were made to match the additional peaks to known compounds. The
results were however inconclusive. The logical source of the additional component is the
binder. Further analysis is required.
33
Figure 24: Prill at 53x Magnification
34
Figure 25: Prill at 1033x Magnification
35
Figure 26: XRD Results
36
5.6 Conclusion
The following conclusions can be made following the analysis of the 'N-Gold' data.
v Coalescence occurs by random and preferential coalescence.
v The moisture content in the system is directly related to the range of the size
distribution at the granulator outlet.
v Much of the fine material that successfully agglomerates is produced in the crushing
and screening stages of the granulation circuit.
v A large number of granules in the size range 0.225mm to 1mm pass through the
granulator without undergoing size enlargement.
5.7 Recycle Ratio Reduction Techniques

It has been identified that the majority of the fine material (0 to 0.225 microns) is
granulated successfully. The intermediate size range of 0.225 to 1mm however has poor
granulation properties. This is largely due to their non-deformable nature resulting in a
tendency to rebound during collisions. It is therefore proposed that to improve the
granulation of 'N-Gold' the urea feed be passed through a grinder. This will have the
effect of increasing the amount of fine material and reduce the intermediate size range.
It has also been identified that the moisture content in the granulator is proportional to the
rate of preferential coalescence. Preferential coalescence has the effect of spreading the
particle size distribution. By controlling the moisture content in the system a suitable
particle distribution spread will maximise the amount of fertilizer in the product size
range.
37
6.0 Granulation Simulation

6.1 Model Development
Simulating the granulation process of 'N Gold' using a mathematical model provides a
useful way to analyse the granulation circuit. By performing a population balance over
the granulation circuit the change in particle size distribution of the fertilizer can be
followed. The simulation package can then be used to better understand the process
operating conditions. In addition a mathematical simulation provides a useful way to
analyse the process control aspects of the granulation circuit.
Jang (1996) developed a Nimbus simulation for a di-ammonium phosphate (DAP)

granulation circuit. The model composed of a granulator, rotary drum drier, vibrating
screen, crusher and conveyor belt. The circuit is controlled by a feedback / feedforward
control loop. Figure 27 shows a block diagram representing the units within the model
and how they are connected.
NH3 Water
Air in
Slurry Granulator Granulator Dry_rate

Reactior Layering Direr
Stage 1 Stage 2
Senf
Sum PI Convey Crusher Screens Product
Senn Belt
Sens
Forward Senr
Seng
Figure 27: Granulation Circuit of Di-Ammonium Phosphate as Modeled by Jang

(1996)
The mechanisms associated with each of the major units within the model are outlined in
appendix 2. This model has been validated on the granulation circuit at Incitec. By
adjusting the model parameters and mechanisms the model has been fitted to the 'N Gold'
process. The following sections of the model developed by Jang are not suitable for the
'N Gold' process and have been removed:
1. The slurry feed of DAP to the granulation drum.
2. The reaction of mono-ammonium phosphate with ammonia in the granulation
drum.
3. The layering of slurry on to the recycled particles.
4. The control loop is not required for the simulation.
38
The following units have been added to the model:

1. A source of urea fines.
2. A mixer to combine the urea fines feed with the recycled product.
Figure 28 shows a block diagram representing the adjusted model.
Air in
Granulator
Urea
Granulator Granulator
Fines Mixer Direr Dry_rate
Stage 1 Stage 2
Feed
Convey Belt Crusher Screens Product
Figure 28: Granulation Circuit for 'N Gold Process
The Nimbus codes for the urea fines source and the mixer are shown in appendix 6.
6.2 Model Fitting - Granulation Drum

The critical part of the granulation circuit is the granulation drum. The granulation drum
has been separated into two stages based on the work of Adetayo et al (1993):
Stage 1: Random coalescence, size independent kernel.
Stage 2: Preferential coalescence, size dependent kernel.
It has been shown in Section 5.2 that both these mechanisms contribute to the granulation
of 'N-Gold'.
There are three areas of the granulation drum model that must be adjusted to fit to the 'N
Gold' process, the particle size distribution, the physical constants and the empirical
constants.
6.2.1 Size Distribution

The size interval used on the 'N-Gold' sampling trials differ from the size interval used to
validate the model on the DAP circuit. The code for the first and second stages of
granulation were adjusted to suit a sieve series used in the 'N-Gold' sampling trials
outlined in section 4.2. The adjusted code is shown in appendix 6.
39
6.2.2 Physical Constants

The granulation model uses the physical constants of the particles in developing the rate
constant for the circuit. The physical constants required for the model are outlined in
Appendix 1. The effect of changing the physical constants on the rate of granulation for
given moisture content has been investigated. The calculation of the rate of granulation
using the properties of 'N-Gold' and di- ammonium phosphate for moisture content of 3%
is shown below.
The rate constant in the granulation drum is given by:
 A1 S sat

β ij =  0 ; S sat < S crit
 A (v + v ) ; S > S
 2 i j sat crit
Where
A1 = Parameter for random kernel ρ f = Density of fertiliser salt
A2 = Parameter for preferential kernel ρl = Density of fertiliser solution
S sat = Fractional saturation of granules p = Particle porosity
S crit = Critical granule saturation X w = Moisture content
vi , v j = Volume of particles S s = Solubility of fertiliser salt in water
The first stage of granulation uses the physical properties to calculate Ssat and therefore
the rate constant. Ssat is given by:
X w ρ f (1 − p )(1 + S s )
S sat =
ρl p(1 − X w S s )
For 'N-Gold' Ssat is:

0.03 * 1.34(1 − 0.35)(1 + 1.19)
S sat =
1.29 * 0.35(1 − 0.03 * 1.19 )
= 0.1315
For DAP Ssat is:

0.03 * 1.5(1 − 0.35)(1 + 0.7)
S sat =
1.3 * 0.35(1 − 0.03 * 0.7 )
= 0.1125
40
The size independent kernel rate constant for both 'N-Gold ' and DAP is therefore given
by:
Rate Constant
'N-Gold' β ij = 0.1315 A1
DAP β ij = 0.1125 A1
For a given value of A1 it can be seen that the rate of the size independent kernel is
greater for 'N-Gold' then for DAP fertilizer. The problem exists however that the
granulation efficiency of 'N-Gold' is smaller then DAP. It is therefore evident that the
empirical constant, A1 , needs to be adjusted to fit the 'N-Gold' process.
6.2.3 Empirical Constants

The performance of the granulation simulation can be adjusted by changing the values of
the empirical constants, A1 and A2 . Figure 29 shows the effect of a change in A1 while
A2 is held constant. Increasing A1 has the effect of increasing the rate of the size
independent kernel mechanism. The figure shows that as A1 is increased a greater
proportion of the fine material (0.053 - 0.125 mm) is consumed. This has the effect of
shifting the size distribution to the right. This is because the as the name suggests the
growth of the particles is independent of size. Therefore the greatest growth occurs in the
fines where there is the greatest amount of particles.
450
400
a1=20
350
a1=45
Mass Flowrate
300 a1=0
250
200
150
100
50
0
0.01 0.1 1 10 100
Size (mm)
Figure 29: Effect of the Size Independent Kernel on Granulation
41
Figure 30 shows the effect of changing A2 while holding A1 constant. This has the effect of
changing the size dependent kernel on granulation. Figure 30 shows that increasing A2
spreads the particle size distribution. This results from the larger particles growing faster
then the smaller particles.
450
400 a2=0.016
a2=0.16
350 a2=1.6
300
Mass Flowrate
250
200
150
100
50
0
0.01 0.1 1 10 100
Size (mm)
Figure 30: Effect of the Size Dependent Kernel on Granulation
These results agree with Adetayo (1993) as shown in Figure 31.
The spikes seen in the particle size distribution at 11mm are a result of the numerical
methods used in the model. The calculations are performed using a number balance. The
results are then converted to a mass balance for the output. In the large size ranges, a
small number of particles will result in a large mass, producing the spike in the
distribution.
Figure 31: Effect of Changing β (u , v )
42
6.3 Model Fitting for the Granulator
Initial Conditions
The first step in fitting the model to the sampled data is providing the necessary initial
conditions. The model requires the particle size distribution in two forms. The first is a
mass flowrate into and out of each of the units in the model. These values can be taken
directly from the sieving results.
Within each stage of the granulator, an orthogonal collocation approach is used to model
the spatial variations. Each stage has been separated into 5 collocation points. The
calculations are performed using a population balance. Therefore the initial conditions at
each of the collocation points is required in the form of the number of particles. The
number of particles can be calculated from the mass of particles using the following
equation:
3
xi / Li
ni =
Σxi / Li
3
Where:
ni = Number fraction in size i
xi = Mass fraction in size i
Li = Mean size of fraction
In addition to the particle size distribution the length of the granulator drum, moisture
content and residence time are also required. Appendix 7 outlines the initial conditions
for Run 1.
Fitting
In fitting the model to the real data, the model was run to steady state and the empirical
constants, A1 and A2 , are varied until a suitable fit to the data could be achieved. The
best possible fit for each of the five runs is shown in figures 32 through 36.
43
400
350 Actual Outlet

Actual Outlet
300 Simulation
Mass Flowrate (kg/h)
250
200
150
100
50
0
0.01 0.1 1 10 100
Size (mm)
Figure 32: Comparison of Actual Results to Simulation, Run 1
400
Actual Outlet
350
Actual Inlet
Mass Flowrate( kg/min)
Simulation
300
250
200
150
100
50
0
0.01 0.1 1 10 100
Size (mm)

450
Actual Outlet
400
MAss Flowrate (kg/min)
Actual Inlet
350 Simulation
300
250
200
150
100
50
0
0.01 0.1 1 10 100
Size (mm)
44
450
400
Mass Flowrate (kg/min)
Actual Outlet
350 Actual Inlet
Si mul ation
300
250
200
150
100
50
0
0.01 0.1 1 10 100
Size (mm)
350
Actual Outlet
300 Actual Inlet
Mass Flowrate (kg/min)
Simulation
250
200
150
100
50
0
0.01 0.1 1 10 100
Size (mm)
It can be seen that there are difficulties in producing accurate simulation fits to the data.
The largest errors lie in the fines region of the distribution. Only the fines in the in the
size range of 0 to 225 microns are sufficiently removed. There is then an increase in the
number of particles in the region of 225 microns to 1mm. This indicates that the fines
are coalescing with other fines but are not attaching / layering to the larger particles in the
distribution. The addition of a layering mechanism to the granulator may provide a better
fit to the data. Under the layering mechanism the fine, unagglomerated particles would
attach to the larger particles in the system.
An additional limitation of the model is the upper limit in the random coalescence
mechanism that exists. Beyond a certain value of a1 the numerical methods within the
model fail. This limits the consumption of fines in the model. The maximum value of
A1 differs for each of the five runs. It is effected by the conditions of the system.
45
Table 4 shows the empirical constants provide the best fit for each of the five runs. It can
be seen that the constant may vary up to 50%. The granulation calculations in the
simulation are largely dependent on the moisture content in the system. Section 5.2
showed that the large fluctuations in the recycle flow resulted in no correlation between
moisture content and extent of granulation. It can therefore not be expected that the
model will accurately predict the changes in the particle size distribution of the sampled
data.
Table 4: Empirical Constants

Run a1 a2
1 45 1.5
2 20 0.5
3 30 0.4
4 40 0.5
5 20 0.7
Figure 37 shows the effect of varying the moisture content by ± 50% on the granulator
outlet size distribution. As the moisture content increases there is a small increase in the
amount of fines removal and a small shift to the right in the size distribution. Apart from
the inlet size distribution the only difference in each of the models is the moisture
content. It is evident that the moisture content is having an insignificant effect on the
particle size distribution.
1400
+50%
1200 2% H2O
Cummulative Mass
-50%
1000
800
600
400
200
0
0.01 0.1 1 10 100
Size (mm)
Figure 37: Effect of Moisture Content on Size Distribution
46
6.4 Conclusion
The validation of the model was limited by errors in the sampling results. It has been
identified that in order to model the 'N-Gold' processes effectively, a series of changes to
the simulation need to be made.
1. Incorporate a layering mechanism into the granulation process.
2. Review the numerical methods of the simulation to allow greater effect of the
random coalescence on granulation.
3. Model the binder flowrate and distribution within the granulation drum.
4. Model the energy balance over the granulation circuit including the energy
input associated with the steam.
47
7.0 Conclusion
The investigation into the granulation of 'N-Gold' has identified that two mechanisms
contribute to its granulation. These mechanisms are random and preferential
coalescence. As the moisture content in the system increases, the range of the granulator
outlet size distribution spreads due to a greater contribution by the preferential
coalescence mechanism. Within the granulator a large proportion of the fine material
below 225 microns is successfully agglomerated. Much of this fine material is produced
during the crushing and screening stages of the circuit.
Image analysis indicates the formation of four different particle types; large agglomerates
in the particle size range; deformagle agglomerates attached to non-deformable crystals;
agglomerates of non-deformable particles; large spherical agglomerates outside the
product size range. In addition there are many particles that pass through the granulator
without undergoing any size enlargement. The majority of these particles are in the
intermediate size range of 0.225mm to 1mm.
X-ray diffraction analysis showed, as expected, that the major component of 'N-Gold' is
urea. There are however additional components within the granules. Attempts were
made to match the additional peaks to known compounds. The results were however
inconclusive. The logical source of the additional component is the binder. Further
analysis is required to identify the non-urea components.
The granulation simulation developed by Jang (1996) was adapted to suit 'N-Gold'
granulation. Both random and preferential coalescence mechanisms were successfully
modeled. The effectiveness the simulation was limited by a combination of the unstable
granulation processes during sampling due to unreliable data and sections of the model
that do not fit 'N-Gold'. It has been identified that to produce a closer fit of experimental
data to the simulation results, the following changes in the model should be made:
5. Incorporate a layering mechanism into the granulation process.
6. Review the numerical methods of the simulation to allow greater effect of the random
coalescence on granulation.
7. Model the binder flowrate and distribution within the granulation drum.
8. Model the energy balance over the granulation circuit including the energy input
associated with the steam.
It has been concluded that the non-deformable particles in the size range of 0.225 mm to
1mm in the urea feed are a major contributing factor to the large recycle ratios. Grinding
the urea fines feed before it is granulated would greatly improve the granulation
efficiency. In addition effective control of the moisture content in the system will ensure
that granulation proceeds by both random and preferential coalescence mechanisms.
48
8.0 NOMENCLATURE
A1 = Parameter for random kernel

A2 = Parameter for preferential kernel
A(v ) = Attrition rate
Bnuc (v) = Nucleation rate
d 953 = 95% passing size of distribution
G (v ) = Layering rate
h = Spread of size distribution
l = Degree of liberation
Li = mean size of fraction
M = Mass from which sample is taken
M s = Mass of sample
N t = Total number of particles per unit volume
ni = number fraction in size I
n = Number of size intervals.
p = Particle porosity
Q = Inlet and exit flowrates from granulator.
r = Effective granule size, m
R = Radius of granulation drum, m
S sat = Fractional saturation of granules
S s = Solubility of fertiliser salt in water
S crit = Critical granule saturation
vi , v j = Volume of particles
V = Volume of granulator
xi = mass fraction in size i
X w = Moisture content
y =Average mass at given size interval
yi = Mass at given size interval
α v = Volume shape factor
β (u , v, t ) = Coalescence kernel
ρ g = Granule density, g/cm3
ρ f = Density of fertiliser salt
ρl = Density of fertiliser solution
µ = Binder Viscosity, P
ω = Drum speed, s-1
49
9.0 References
Adetayo, A. A. and Ennis, B. J., 1997. 'Unifying Approach to Modeling Granule
Coalescence Mechanisms', AIChE Journal, 43(4), pp.927-934.
Adetayo, A. A., Litster, J.D. and Cameron, I.T., 1995. 'Steady State Modelling and
Simulation of a Fertilizer Granulation Circuit, Computers chem. Engng, 19(4), pp. 383-
393.
Adetayo, A. A., Litster, J.D. and Desai, M., 1993. 'The Effect of Process Parameters on
Drum Granulation of Fertilizers with Broad Size Distributions', Chemical Engineering
Science, 48(23), pp.3951-3961.
Bathala C. R., Dodlaty V. S. M., Madaboosi, S.A. and Chamarti D.P.R., 1993. 'Modeling
of Continuous Fertilizer Granulation Process for Control', Particle Particle System
Characterization, 15, pp. 156-160.
Davis, G., 1996, Collection of Granulation Circuit Data for Plant Evaluation and
Simulation, Undergraduate Thesis, Department of Chemical Engineering, University of
Queensland.
Ennis, B. J., 1996. 'Agglomeration and size enlargement Session summary paper',
Powder Technology, 88, pp. 203-225.
Iverson, S.M. and Litster, J.D., 1998, Growth Regime Map for Liquid-Bound Granules,
Powder Technology and Fluidization, 44 (7), pp. 1510-1518.
Iveson, S.M., Litster, J.D. and Ennis, B.J., 1996, 'Fundamental studies of granule
consolidation Part 1: Effects of binder content and binder viscosity', Powder Technology,
88, pp. 15-20.
Litster, J.D. and Sarwono. R., 1996. 'Fluidized drum granulation: studies of agglomerate
formation', Powder Technology, 88, pp. 165-172.
Reddy, B.C., Murthy, D.V.S. and Rao, C.D.P., 1997, 'Continous Rotary Drum
Granulation of N-K Fertilizers', Part. Part. Syst. Charact. 14, pp. 257-262.
Sherington, P.J., (1968), The Chemical Engineer, pp. 201.
Smith, R and James, G.V., 1981, The Sampling of Bulk Materials, London: Royal
Society of Chemistry.
Snow, R.H., Allen, T., Ennis, B.J. and Litster, J.D., 1997, 'Size reduction and Size
Enlargement', Perry's Chemical Engineers Handbook, 7, pp. 20-56 to 20-89.
50
Zhang, J., 1996, Dynamics and Control of Fertilizer Granulation Circuit, Postgratuate
Thesis, Department of Chemical Engineering, University of Queensland.
Hounslow, M.J. and Ryall, R.L. and Marshall, V.R., 1988, A Discretized Population
Balance for Nucleation, Growth, and Aggregation, AIChE, 34 (11), pp. 1821-1832.
Ennis, B.J., Tardos, G. and Pfeffer, R., 1991, A Microlevel-Based Characterization of

Granulation Phenomena, Powder Technology, 65, pp. 257-272.
51
APPENDIX 1
'N-Gold' Properties
Table 1 shows a comparison of the properties of 'N-Gold' and the other fertilizers produced at
Incitec.
Table 1: Physical Properties of Fertilizer
Urea AS MAP DAP
True Density (g/cm3) 1.34 1.7 1.6 1.5
Solubility 119 78 46 75
(g/ml)
Density of fertilizer 1.29 1.3
Solution(ρl, g/cm3)
Solubility (Ss, g/ml) 1.19 0.7
Porosity of Granule 0.35 0.35
(p)
Viscosity 3.4 3.7 8.5
52
APPENDIX 2
Dynamic Fertilizer Model
Zhang (1996) has developed a dynamic model for the granulation of di-ammonium phosphate.
This model was adapted from the steady state model developed by Adetayo et al. (1995). The
model includes the granulation drum, drier, screen, and crusher.
Granulation Drum
A dynamic model of the granulation drum has been developed that uses Hounslow's descritized
population balance and the two-stage coalescence kernel proposed by Ennis [10]. (See section
2.1). The coalescence kernel is given by:
 AS sat

β ij =  0 ; S sat < S crit
k (v + v ) ; S > S
 2 i j sat crit
In the development of the model, the assumptions have been made that no particle breakage
occurs and that the operating temperature is constant along the drum.
Incorporated in to the granulation drum model is the reaction between mono-ammonium

phosphate and ammonia to give di-ammonium phosphate.
Drier
A distributed parameter model of a rotary drum drier has been used. The model describes the
behaviour under co-current conditions. The key assumption in the development of the drier
model is that there is no particle breakage or granulation occurring within the drier.
The accuracy of the assumption will be tested through the analysis of the particle size
distributions before and after the drier in the N-Gold process.
Screen
The screen model is based on the probability that a particle will pass through the aperture of the
screen.
Crusher
A matrix model has been used to model the crusher; this was validated for fertilizer processes by
Adetayo [1]. The key assumptions of the model are:
v Single fracture breakage occurs
v The breakage is assumed to be constant within a size interval
v The system is assumed to be perfectly mixed
v Efficiency is not a function of flowrate.
The input data requirements for each of the units are shown below.
Granulator Drier Crusher / Screen

Particle Size Distribution Air Flowrate Solid Flowrate
Solid Flowrate Solid Flowrate Particle Size Distribution
Binder Flowrate Moisture Content
Water Content Temperature
Input Requirements for Granulation Circuit
53
APPENDIX 3
Sampling Error Calculations
Density 1.34
D95
Run 1 2.5
Run 2 1.94
Run 3 4.2
Run 4 4
Run 5 3.6
Run 1 Run 2 Run 3 Run 4 Run 5

Sieve Mass on Mass Mass on Mass Mass on Mass Mass on Mass Mass on Mass
Size Sieve Fraction Sieve Fraction Sieve Fraction Sieve Fraction Sieve Fraction
11.2 0 0 2.35 0.01136 2.35 0.011624 0 0

8 0 0 2.76 0.013342 2.76 0.013653 0.55 0.00186
5.6 0.87 0.004175 0.85 0.003848 7.27 0.035143 7.27 0.035962 5.84 0.01978
4 5.13 0.024621 0.7 0.003169 12.67 0.061246 12.67 0.062673 28.19 0.09548
2.8 14.09 0.067623 6.01 0.027209 21.04 0.101706 21.04 0.104076 51.86 0.17566
2 35.21 0.168986 59.35 0.268698 41.8 0.202059 41.8 0.206767 59.9 0.20289
1.4 67.49 0.323911 81.02 0.366806 59.96 0.289844 59.96 0.296597 67.7 0.22931
1 38.65 0.185496 36.38 0.164705 32.2 0.155653 32.2 0.15928 32.76 0.11096
0.71 22.25 0.106786 18.31 0.082896 13.3 0.064292 13.3 0.065789 20.97 0.07103
0.5 12.18 0.058457 8.64 0.039116 5.32 0.025717 5.32 0.026316 12.71 0.04305
0.335 6.77 0.032492 4.71 0.021324 1.66 0.008024 1.66 0.008211 6.94 0.02351
0.25 3.06 0.014686 2.33 0.010549 5.5 0.026587 0.79 0.003908 4.24 0.01436
0.18 0.98 0.004703 0.78 0.003531 0.36 0.00174 0.36 0.001781 1.5 0.00508
0.125 0.38 0.001824 0.63 0.002852 0.22 0.001063 0.22 0.001088 0.86 0.00291
0.09 0.7 0.00336 0.53 0.002399 0.17 0.000822 0.17 0.000841 0.61 0.00207
0.053 0.37 0.001776 0.41 0.001856 0.2 0.000967 0.2 0.000989 0.53 0.0018
0 0.23 0.001104 0.23 0.001041 0.09 0.000435 0.09 0.000445 0.07 0.00024
Total 208.36 1 220.88 1 206.87 1 202.16 1 295.23
Error 7.01 4.64 14.25 15.53 9.90
Granulator Exit Cumulative Plot
1.1
1
0.9
0.8
0.7 Run 1
Mass
0.6 Run 2
0.5 Run 3
0.4 Run 4
0.3 Run 5
0.2
0.1
0
0 2 4 6 8 10 12
Size (mm)
54
APPENDIX 4
Error Calculations for Precision Analysis
Test A Test B Test C Test D ybar Standard Error
Deviation
11.2 0 0 0 0 0 0 0 0 0 0 0
8 0.0079 0 0 0.00209 0.0025 2.9E-05 6.2E-06 6.2E-06 1.7E-07 0.003734 0.74674
5.6 0.0036 0.00147 0.00503 0.00315 0.0033 8.4E-08 3.4E-06 2.9E-06 2.6E-08 0.001465 0.292936
4 0.0122 0.00634 0.02806 0.01273 0.0148 7E-06 7.2E-05 0.00017 4.4E-06 0.00928 1.856067
2.8 0.0235 0.01833 0.02077 0.03042 0.0233 7.1E-08 2.4E-05 6.2E-06 5.1E-05 0.005222 1.044363
2 0.0944 0.08012 0.09277 0.12018 0.0969 6E-06 0.00028 1.7E-05 0.00054 0.016801 3.360297
1.4 0.3079 0.26485 0.30472 0.31299 0.2976 0.00011 0.00107 5E-05 0.00024 0.022108 4.421538
1 0.2218 0.20524 0.21474 0.20477 0.2116 0.0001 4.1E-05 9.6E-06 4.7E-05 0.008189 1.63781
0.71 0.1133 0.11086 0.11381 0.10208 0.11 1.1E-05 7.4E-07 1.4E-05 6.3E-05 0.005435 1.08693
0.5 0.0686 0.0769 0.07371 0.06115 0.0701 2.1E-06 4.6E-05 1.3E-05 8E-05 0.006868 1.37363
0.335 0.0378 0.04686 0.04223 0.03321 0.04 5E-06 4.7E-05 4.9E-06 4.6E-05 0.00586 1.171925
0.25 0.0191 0.01686 0.0192 0.01768 0.0182 7.4E-07 1.8E-06 9.9E-07 2.6E-07 0.001124 0.224831
0.18 0.0265 0.04092 0.01246 0.02569 0.0264 7.4E-09 0.00021 0.00019 4.8E-07 0.011628 2.325596
0.125 0.0216 0.04263 0.02583 0.02411 0.0285 4.8E-05 0.0002 7.4E-06 2E-05 0.009557 1.911354
0.09 0.0163 0.03307 0.01843 0.01874 0.0216 2.9E-05 0.00013 1E-05 8.3E-06 0.007705 1.540912
0.053 0.014 0.02991 0.01564 0.01685 0.0191 2.6E-05 0.00012 1.2E-05 5.1E-06 0.007297 1.459336
0 0.0115 0.02562 0.01263 0.01415 0.016 2E-05 9.3E-05 1.1E-05 3.4E-06 0.006514 1.302803
Average 1.515122
Error
55
APPENDIX 5
Raw Data - 'N-Gold' Mass Fractions
Urea Fines Granulator Exit
Run 1 Run 2 Run 3 Run 4 Run 5 Run 1 Run 2 Run 3 Run 4 Run 5
11.2 0.000 0.000 0.004 0.020 0.000 11.2000 0.0000 0.0000 0.0135 0.0114
8 0.001 0.002 0.003 0.020 0.000 8.0000 0.0000 0.0000 0.0253 0.0133 0.0019
5.6 0.002 0.004 0.006 0.051 0.001 5.6000 0.0042 0.0038 0.0128 0.0351 0.0198
4 0.007 0.008 0.007 0.028 0.002 4.0000 0.0246 0.0032 0.0339 0.0612 0.0955
2.8 0.137 0.015 0.019 0.037 0.008 2.8000 0.0676 0.0272 0.1040 0.1017 0.1757
2 0.310 0.222 0.219 0.185 0.110 2.0000 0.1690 0.2687 0.2154 0.2021 0.2029
1.4 0.178 0.334 0.334 0.286 0.269 1.4000 0.3239 0.3668 0.3208 0.2898 0.2293
1 0.063 0.155 0.150 0.149 0.144 1.0000 0.1855 0.1647 0.1462 0.1557 0.1110
0.71 0.060 0.072 0.069 0.085 0.107 0.7100 0.1068 0.0829 0.0748 0.0643 0.0710
0.5 0.050 0.046 0.052 0.108 0.067 0.5000 0.0585 0.0391 0.0258 0.0257 0.0431
0.335 0.080 0.037 0.071 0.023 0.073 0.3350 0.0325 0.0213 0.0125 0.0080 0.0235
0.25 0.080 0.043 0.040 0.008 0.100 0.2500 0.0147 0.0105 0.0060 0.0266 0.0144
0.18 0.033 0.046 0.023 0.000 0.108 0.1800 0.0047 0.0035 0.0030 0.0017 0.0051
0.125 0.001 0.013 0.001 0.000 0.010 0.1250 0.0018 0.0029 0.0020 0.0011 0.0029
0.09 0.000 0.003 0.000 0.000 0.000 0.0900 0.0034 0.0024 0.0027 0.0008 0.0021
0.053 0.001 0.000 0.000 0.000 0.000 0.0530 0.0018 0.0019 0.0010 0.0010 0.0018
0 0.000 0.000 0.000 0.000 0.0000 0.0011 0.0010 0.0000 0.0004 0.0002
Granulator Entrance Drier Exit

Run 1 Run 2 Run 3 Run 4 Run 5 Run 1 Run 2 Run 3 Run 4
11.2 0.000 0.000 0.000 0.052 0.000 11.2 0.000 0.000 0.000 0.000
8 0.000 0.000 0.001 0.002 0.000 8 0.003 0.001 0.002 0.020
5.6 0.001 0.001 0.011 0.008 0.004 5.6 0.005 0.007 0.060 0.051
4 0.001 0.002 0.008 0.012 0.045 4 0.026 0.007 0.057 0.028
2.8 0.004 0.005 0.025 0.029 0.100 2.8 0.102 0.030 0.108 0.037
2 0.055 0.085 0.104 0.119 0.152 2 0.148 0.206 0.239 0.186
1.4 0.211 0.351 0.318 0.352 0.258 1.4 0.361 0.283 0.303 0.288
1 0.209 0.227 0.185 0.195 0.130 1 0.189 0.184 0.127 0.149
0.71 0.137 0.110 0.120 0.091 0.077 0.71 0.082 0.103 0.053 0.085
0.5 0.101 0.068 0.054 0.045 0.052 0.5 0.044 0.070 0.021 0.108
0.34 0.078 0.050 0.037 0.022 0.041 0.335 0.022 0.048 0.007 0.023
0.25 0.063 0.041 0.038 0.020 0.039 0.25 0.011 0.038 0.018 0.023
0.18 0.037 0.021 0.041 0.017 0.029 0.18 0.003 0.013 0.002 0.000
0.13 0.033 0.009 0.043 0.013 0.036 0.125 0.001 0.005 0.001 0.000
0.09 0.025 0.016 0.012 0.010 0.016 0.09 0.001 0.004 0.001 0.000
0.05 0.028 0.008 0.002 0.008 0.014 0.053 0.001 0.002 0.001 0.000
0 0.018 0.006 0.000 0.005 0.006 0 0.000 0.001 0.000 0.000
56
APPENDIX 6
Simulation Code
(Code was developed by Jang (1996). Changes have been made to suit the 'N-Gold'
process.)
Urea Fines Source

function_block U-Fines
(* global variables declaration *)
var_external
initialization : bool ; (* enables user code at time zero *)
time : real ; (* simulation time *)
max_time : real ; (* time for end of simulation *)
print_level : int ; (* degree of print output *)
error_tolerance : real ; (* integration error acceptable *)
no_comps : int ; (* number of components *)
end_var
(* global data type declarations *)
type
stream : (* mass flow streams *)

structure
pressure : real ;
temperature : real ;
z_flow : array (1 .. no_comps) of real ;
end_structure ;
energy : (* energy stream *)

structure
z_rate : real ;
end_structure ;
signal : (* information signal *)

structure
z_value : real ;
end_structure ;
end_type
var_in_out
o1 : Stream ; (* feed *)
end_var
var_input
x: array (1 .. 21) of real;
term: real;
end_var
var
i: int;
end_var
var_output
resid_1: array (1 .. 21) of real;
end_var
function error (errcode: int;) end_function
for i:=1 to 21 do
resid_1(i):=x(i)-o1.z_flow(i);
end_for
end_function_block
Granulator Stage 1
function_block granu1
var_external
57
end_var
type

structure
pressure : real ;
end_structure ;

structure
z_rate : real ;
end_structure ;

structure
z_value : real ;
end_structure ;
end_type
var_in_out
i1: stream;
o1: stream;
end_var
var_input
x_n2: array(1 .. 20) of real;
x_xw: array(1 .. 5) of real;
length: real;
tr: real;
densty: real;
end_var
var_output
resid_out: array(1 .. 21) of real;
deriv_n2: array(1 .. 20) of real;
deriv_xw: array(1 .. 20) of real;
end_var
var
a1: array(1 .. 5) of real;
i: int;
j: int;
sum1: real;
sum2: real;
sum3: real;
sum4: real;
beta: array(1 .. 5) of real;
ntotal1: real;
ntotal2: real;
ntotal3: real;
58
ntotal4: real;
ntotal5: real;
mntotal1: real;
mntotal2: real;
mntotal3: real;
mntotal4: real;
mntotal5: real;
dmntotal2: real;
dmntotal3: real;
dmntotal4: real;
dmntotal5: real;
d: array (1 .. 20) of real;
meand: array (1 .. 5) of real;
in_fi: array(1 .. 20) of real;
in_f: array(1 .. 20) of real;
out_fi: array(1 .. 20) of real;
out_f: array(1 .. 20) of real;
dbar: array(1 .. 20) of real;
end_var
function error(errcode: int;) end_function
(* program for birth death rate calculation*)
a1(1):=0.0-13.0/length ;
a1(2):=14.78831/length;
a1(3):=0.0-2.66667/length;
a1(4):=1.87836/length;
a1(5):=0.0-1.0/length;
a2(1):=0.0-5.32378/length;
a2(2):=3.87298/length;
a2(3):=2.06559/length;
a2(4):=0.0-1.29099/length;
a2(5):=0.67621/length;
a3(1):=1.50000/length;
a3(2):=0.0-3.22749/length;
a3(3):=0.0;
a3(4):=3.22749/length;
a3(5):=0.0-1.50/length;
a4(1):=0.0-0.67621/length;
a4(2):=1.29099/length;
a4(3):=0.0-2.06559/length;
a4(4):=0.0-3.87298/length;
a4(5):=5.32379/length;
a5(1):=1.00/length;
a5(2):=0.0-1.87836/length;
a5(3):=2.66667/length;
a5(4):=-14.78831/length;
a5(5):=13.000/length;
d(1):=0.053;
d(2):=0.09;
d(3):=0.125;
d(4):=0.18;
d(5):=0.25;
d(6):=0.335;
d(7):=0.5;
d(8):=0.71;
d(9):=1;
d(10):=1.4;
d(11):=2;
d(12):=2.8;
d(13):=4.0;
d(14):=5.6;
d(15):=8;
d(16):=11.2;
d(17):=12.7;
d(18):=16;
d(19):=20.16;
d(20):=25;
for i:=1 to 20 do
if i==1 then
dbar(i):=(d(i)+0.198)/2;
else
dbar(i):=(d(i)+d(i-1))/2;
59
end_if
end_for
beta(1):= i1.z_flow(21)*(1.0+1.19)*1.34/(1.0-
i1.z_flow(21)*1.19)/1.29*(1.0-0.38)/0.38*6 ;
for i:=2 to 5 do
beta(i):= x_xw(i)*(1.0+1.19)*1.34/(1.0-
x_xw(i)*1.19)/1.29*(1.0-0.38)/0.38*6 ;
end_for
ntotal1:=i1.z_flow(1)-i1.z_flow(1);
mntotal1:=i1.z_flow(1)-i1.z_flow(1);
meand(1):=i1.z_flow(1)-i1.z_flow(1);
for i:=1 to 20 do
ntotal1:=ntotal1+i1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3);
ntotal2:=ntotal2+x_n2(i);
mntotal1:=mntotal1+i1.z_flow( i);
mntotal2:=mntotal2+x_n2(i)/tr*length*densty*(3.14/6*dbar(i)**3);
end_for
for i:=1 to 20 do
meand(1):=meand(1)+i1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)
/ntotal1*dbar( i);
meand(2):=meand(2)+x_n2(i)/ntotal2*dbar(i);
if i==1 then
in_fi(i):=i1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)/ntotal1
/(d(i));
in_f(i):=i1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)/ntotal1;
out_fi(i):=o1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)/ntotal5
/(d(i));
out_f(i):=o1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)/ntotal5;
else
in_fi(i):=i1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)
/ntotal1/(d(i)-d(i-1));
in_f(i):=in_f(i-1)+i1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)
/ntotal1;
out_fi(i):=o1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)
/ntotal5/(d(i)-d(i-1));
out_f(i):=out_f(i-1)+o1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3)
/ntotal5;
end_if
end_for
for i:=1 to 20 do
sum1:=x_n2(i)-x_n2(i);
if i > 1 then
sum1:= sum1+0.5*beta(2)
*x_n2(i-1)*(x_n2(i-1));
*x_n3(i-1)*(x_n3(i-1));
60
*x_n4(i-1)*(x_n4(i-1));
*x_n5(i-1)*(x_n5(i-1));
end_if
for j:=1 to 20 do
if j <= i-2 then
sum1:=sum1+2.0**(j-i+1)*beta(2)
*x_n2(i-1)*x_n2(j) ;
sum2:=sum2+2.0**(j-i+1)*beta(3)
*x_n3(i-1)*x_n3(j) ;
sum3:=sum3+2.0**(j-i+1)*beta(4)
*x_n4(i-1)*x_n4(j) ;
sum4:=sum4+2.0**(j-i+1)*beta(5)
*x_n5(i-1)*x_n5(j) ;
end_if
if j <= i-1 then
sum1:= sum1-2.0**(j- i)*beta(2)
*x_n2(i)*x_n2(j);
sum2:= sum2-2.0**(j- i)*beta(3)
*x_n3(i)*x_n3(j);
sum3:= sum3-2.0**(j- i)*beta(4)
*x_n4(i)*x_n4(j);
sum4:= sum4-2.0**(j- i)*beta(5)
*x_n5(i)*x_n5(j);
else
sum1:= sum1-beta(2)
*x_n2(i)*x_n2(j);
sum2:= sum2-beta(3)
*x_n3(i)*x_n3(j);
sum3:= sum3-beta(4)
*x_n4(i)*x_n4(j);
sum4:= sum4-beta(5)
*x_n5(i)*x_n5(j);
end_if
end_for
deriv_n2(i):=0.0-(a2(1)*i1.z_flow(i)
*tr/length/ densty/(3.14/6*dbar(i)**3)
+a2(2)*x_n2( i)
+a2(3)*x_n3( i)+a2(4)*x_n4(i)
+a2(5)*x_n5( i))*length/tr
+sum1/ntotal2;
+a3(2)*x_n2( i)
+a3(3)*x_n3( i)+a3(4)*x_n4(i)
+sum2/ntotal3;
+a4(2)*x_n2( i)
+a4(3)*x_n3( i)+a4(4)*x_n4(i)
+sum3/ntotal4;
+a5(2)*x_n2( i)
+a5(3)*x_n3( i)+a5(4)*x_n4(i)
+sum4/ntotal5;
resid_out(i):= x_n5(i)*length/tr*densty*(3.14/6*dbar(i)**3)
-o1.z_flow(i);
end_for
dmntotal2:=0.0-(a2(1)*mntotal1+a2(2)*mntotal2
+a2(3)*mntotal3+a2(4)*mntotal4
+a2(5)*mntotal5)*length/tr;
61
deriv_xw(2):=0.0-((a2(1)*i1.z_flow(21)*mntotal1
+a2(2)*x_xw(2)*mntotal2
+a2(5)*x_xw(5)*mntotal5)*length/tr
+x_xw(2)*dmntotal2)/mntotal2;
resid_out(20+1):=x_xw(5)-o1.z_flow(20+1);
end_function_block
Granulator Stage 2
function_block try
var_external

end_var
type

structure
pressure : real ;
end_structure ;

structure
z_rate : real ;
end_structure ;

structure
z_value : real ;
end_structure ;
end_type
62
var_in_out
i1: stream;
o1: stream;
o2: signal;
end_var
var_input
x_xw: array(1 .. 5) of real;
length: real;
tr: real;
densty: real;
constn: real;
end_var
var_output
resid_1: array(1 .. 21) of real;
resid_2: real;
deriv_xw: array(1 .. 5) of real;
end_var
var
i: int;
j: int;
ii: int;
sum1: real;
sum2: real;
sum3: real;
sum4: real;
term: real;
ntotal1: real;
ntotal2: real;
ntotal3: real;
ntotal4: real;
ntotal5: real;
mntotal1: real;
mntotal2: real;
mntotal3: real;
mntotal4: real;
mntotal5: real;
psum: real;
sum: real;
d: array(1 .. 20) of real;
meand: array(1 .. 5) of real;
fi: array(1 .. 20) of real;
f: array(1 .. 20) of real;
dbar: array(1 .. 20) of real;
tn: real;
end_var
function error(errcode: int;) end_function
(* program for birth death rate calculation*)
a1(1):=0.0-13.0/length ;
a1(2):=14.78831/length;
a1(3):=0.0-2.66667/length;
a1(4):=1.87836/length;
a1(5):=0.0-1.0/length;
a2(1):=0.0-5.32378/length;
a2(2):=3.87298/length;
a2(3):=2.06559/length;
a2(4):=0.0-1.29099/length;
a2(5):=0.67621/length;
a3(1):=1.50000/length;
63
a3(2):=0.0-3.22749/length;
a3(3):=0.0;
a3(4):=3.22749/length;
a3(5):=0.0-1.50/length;
a4(1):=0.0-0.67621/length;
a4(2):=1.29099/length;
a4(3):=0.0-2.06559/length;
a4(4):=0.0-3.87298/length;
a4(5):=5.32379/length;
a5(1):=1.00/length;
a5(2):=0.0-1.87836/length;
a5(3):=2.66667/length;
a5(4):=-14.78831/length;
a5(5):=13.000/length;
d(1):=0.053;
d(2):=0.09;
d(3):=0.125;
d(4):=0.18;
d(5):=0.25;
d(6):=0.335;
d(7):=0.5;
d(8):=0.71;
d(9):=1;
d(10):=1.4;
d(11):=2;
d(12):=2.8;
d(13):=4.0;
d(14):=5.6;
d(15):=8;
d(16):=11.2;
d(17):=12.7;
d(18):=16;
d(19):=20.16;
d(20):=25;
for i:=1 to 20 do
if i==1 then
dbar(i):=(d(i)+0.198)/2;
else
dbar(i):=(d(i)+d(i-1))/2;
end_if
end_for
sum:=i1.z_flow(1)-i1.z_flow(1);
psum:=i1.z_flow(1)-i1.z_flow(1);
for i:=1 to 20 do
sum:=sum+o1.z_flow(i);
end_for
for i:=10 to 13 do
psum:=psum+o1.z_flow(i);
end_for
ii:= i1.z_flow(1)-i1.z_flow(1);
(* for j:=1 to 20 do
for i:=1 to 20 do
ii:=ii+1;
beta(20*(j-1)+i):= 0.0156*constn*(2**(i-0.5)+2**(j-0.5)) ;
end_for
end_for*)
tn:= i1.z_flow(1)-i1.z_flow(1);
for i:=1 to 20 do
ntotal1:=ntotal1+i1.z_flow(i)*tr/length/densty/(3.14/6*dbar(i)**3);
64
mntotal1:=mntotal1+i1.z_flow( i);
tn:=tn+x_n5(i)/tr*length;
end_for
for i:=1 to 20 do
if i==1 then
fi(i):=x_n5(i)/ntotal5/(d(i));
f(i):=x_n5(i)/ntotal5;
else
fi(i):=x_n5(i)/ntotal5/(d(i)-d(i-1));
f(i):=f(i-1)+x_n5(i)/ntotal5;
end_if
end_for
for i:=1 to 20 do
if i > 1 then
sum1:= sum1+0.5*$Rate*3.14/6*( dbar(i-1)**3+dbar(i-1)**3)
*x_n2(i-1)*(x_n2(i-1));
sum2:= sum2+0.5*$Rate *3.14/6*( dbar(i-1)**3+dbar(i-1)**3)
*x_n3(i-1)*(x_n3(i-1));
*x_n4(i-1)*(x_n4(i-1));
*x_n5(i-1)*(x_n5(i-1));
end_if
for j:=1 to 20 do
if j <= i-2 then
sum1:=sum1+2.0**(j-i+1)* $Rate *3.14/6*( dbar(j)**3+dbar(i-1)**3)
*x_n2(i-1)*x_n2(j) ;
*x_n3(i-1)*x_n3(j) ;
*x_n4(i-1)*x_n4(j) ;
*x_n5(i-1)*x_n5(j) ;
end_if
if j <= i-1 then
sum1:= sum1-2.0**(j- i)* $Rate *3.14/6*(dbar(j)**3+dbar(i)**3)
*x_n2(i)*x_n2(j);
*x_n3(i)*x_n3(j);
*x_n4(i)*x_n4(j);
*x_n5(i)*x_n5(j);
else
sum1:= sum1-$Rate *3.14/6*( dbar(j)**3+dbar(i)**3)
*x_n2(i)*x_n2(j);
*x_n3(i)*x_n3(j);
*x_n4(i)*x_n4(j);
*x_n5(i)*x_n5(j);
end_if
end_for
term:=1.0;
deriv_n2(i):=0.0-(a2(1)*i1.z_flow(i)*term
+a2(2)*x_n2( i)
+a2(3)*x_n3( i)+a2(4)*x_n4(i)
+sum1/ntotal2;
65
+a3(2)*x_n2( i)
+a3(3)*x_n3( i)+a3(4)*x_n4(i)
+sum2/ntotal3;
+a4(2)*x_n2( i)
+a4(3)*x_n3( i)+a4(4)*x_n4(i)
+sum3/ntotal4;
+a5(2)*x_n2( i)
+a5(3)*x_n3( i)+a5(4)*x_n4(i)
+sum4/ntotal5;
resid_1(i):= x_n5(i)/term*length/tr*densty*(3.14/6*dbar(i)**3)
-o1.z_flow(i);
end_for
for i:=1 to 20 do
(* meand(1):=meand(1)+i1.z_flow(i)*d(i)/mntotal1;
meand(2):=meand(2)+x_n2(i)/tr*length
*densty*(3.14/6*dbar(i)**3)*d(i)/mntotal2;
*densty*(3.14/6*dbar(i)**3)*d(i)/mntotal3;
*densty*(3.14/6*dbar(i)**3)*d(i)/mntotal4;*)
meand(5):=meand(5)+x_n5(i)/tr*length*dbar(i)/tn;
end_for
deriv_xw(2):= (a2(1)*i1.z_flow(20+1)+a2(2)* x_xw(2)+a2(3)*x_xw(3)
+a2(4)*x_xw(4)+a2(5)*x_xw(5))*(0.0-length/tr);
resid_1(20+1):=x_xw(5)-o1.z_flow(20+1);
(* resid_2:=o2.z_value-x_xw(5);*)
end_function_block
66
APPENDIX 7
Initial Conditions - Granulator
Collocation Points
Granulator
Stage 1 Stage 2
1 2 3
A B C D E F G H I J
Mass of Number of
Particles Particles
1 2 3A B C D E F G H I J
11.2 5.234 2.775 1.136
8 0.224 0.890 1.334 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000
5.6 0.765 2.415 3.514 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000
4 1.224 4.164 6.125 0.000 0.000 0.000 0.000 0.001 0.001 0.001 0.001 0.001 0.001
2.8 2.932 7.275 10.171 0.001 0.002 0.002 0.003 0.004 0.005 0.005 0.006 0.007 0.008
2 11.870 16.872 20.206 0.009 0.015 0.021 0.027 0.033 0.039 0.046 0.052 0.058 0.064
1.4 35.191 31.467 28.984 0.067 0.098 0.128 0.159 0.190 0.220 0.251 0.281 0.312 0.342
1 19.471 17.127 15.565 0.157 0.226 0.296 0.366 0.435 0.505 0.575 0.645 0.714 0.784
0.71 9.109 7.501 6.429 0.263 0.371 0.479 0.587 0.695 0.803 0.911 1.019 1.127 1.235
0.5 4.526 3.353 2.572 0.462 0.625 0.788 0.950 1.113 1.275 1.438 1.600 1.763 1.926
0.34 2.160 1.345 0.802 0.731 0.909 1.086 1.263 1.441 1.618 1.795 1.972 2.150 2.327
0.25 1.957 2.378 2.659 6.903 11 15.040 19 23 27 31 35.4 39.5 43.5
0.18 1.651 0.765 0.174 7.450 8 7.730 8 8 8 8 8.4 8.6 8.7
0.13 1.292 0.580 0.106 20.3 20 19.973 20 20 20 19 19.3 19.1 19.0
0.09 1.035 0.463 0.082 72.6 72 71.091 70 70 69 68 67.3 66.6 65.8
0.05 0.826 0.388 0.097 194.1 200 206.3 212 218 225 231 236.7 242.8 248.9
0 0.534 0.240 0.044 1653.8 1641 1627.6 1614 1601 1588 1575 1562.1 1549.0 1536.0
Granulator
Stage 1 Stage 2
Moisture Content 0.02 0.02
Granulator Length 1 7
Granulator Residence Time 0.625 4.375
67

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Thesis David Brooker

Improving Granulation Techniques

Department of Chemical Engineering

5.2 Results of 'N-Gold' Data Collection 23

Appendix 1 Physical Properties of Fertilisers 51

Appendix 2 Granulation Simulation 52

Appendix 3 Sampling Error 53

Appendix 4 Precision of Sampling 54

Appendix 5 Raw Data 55

Appendix 6 Nimbus Code 51

Appendix 7 Granulator Initial Conditions 66

Figure 1: 'N-Gold' Granulation Circuit

The granulation circuit poses two main problems:

1.2 Thesis Objectives

v Perform a plant audit on the 'N-Gold' granulation process

v Analyse the data using a range of particle characterization techniques

v Simulate the 'N-Gold' granulation circuit using existing modeling facilities

2.0 LITERATURE REVIEW

Figure 2: Major Granulation Mechanisms

Experimental observations of granulation processes indicate that the mechanisms of size

2. The second factor effecting the granulation of fertilizers is their solubility.

Appendix 1 summarizes the physical characteristics of a range of fertilizer compounds. It

2. When sufficient moisture is provided a second stage of granulation occurs called

An alternative approach to modeling fertilizer granulation mechanisms was developed by

2.2 Effects of Binder Content and Viscosity on Granulation

Pendular Funicular Capillary

2.3 Effect of Initial Size Distribution

2.4 Effect of Circuit Performance on Granulation

2.5 Granulation Modeling and Simulation

∂n(v, t ) Qin Q ∂(G * − A*)n(v.t )

∫ β (u, v − u, t )n(u, t )n(v − u, t )du

In general this population balance cannot be solved by analytical methods. It is therefore

Recent research has identified improvements in the modeling of granulation of fertilizers.

An alternative approach to modeling a dynamic fertilizer granulation process was

2.6 'N-Gold' Analysis

2.7 Scope of Work

3.0 PLAN OF STUDY

Table 1: Data Requirements

3.2 Quantity of Samples

3.2 Sample Analysis

The following analysis has been performed on the samples:

3.3 Model Fitting and Simulation

3.3.1 Model Development

3.3.2 Model Fitting

4.0 EXPERIMENTAL PROCEDURE

Figure 5: Sampling Points

4.1.1 Sampling Procedures

In order to take a representative sample the following rules should be followed:

v A powder should always be sampled while in motion.

It is therefore necessary to design the correct sampling equipment to obtain a

Figure 6: A - Granulator exit sampler; B - General purpose sampling device

4.2 Size Analysis

The factors effecting the accuracy of sieving are:

The amount of separation achieved is a function of the sieving time. By maintaining a

Figure 7: Sieve Shaker

4.2.1Particle Size Analysis Procedure

4.3 Moisture Content Analysis

4.4 Image Analysis

Figure 8: Camera used for Image Analysis

4.4.3 Electron Scanning Microscope

4.5 X-Ray Diffraction

5.0 Results / Discussion