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To Copy to
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4 Snamprogetti worldwide Urea Users
Symposium

Title

Urea Granulation Technology

Summary

Urea granulation technology has reached a stage where economy of scale and operational reliability are
the key success factors. Being the tail of a multi million-dollar investment, margins between success and
failure are small.

The relevant fundamentals of granulation technology are favouring different techniques for different
products and starting points. The key to success is combining unit operations in order to recover or utilise
various forms of energy being available.

In Urea Granulation, the first key to success is combining the heat of evaporation with heat of
crystallisation of the urea. This combination is easier said than done. Granulation of urea with high water
content in the incoming solution is only possible with a fine-tuning of the whole process.

This paper is handling a few key issues in a technique orientation, and is not an attempt to benchmark the
present technologies in the market.

The development of the present Yara technology is not a by-product or spin-off, but a long-term dedicated
effort requiring large investment in facilities and people, and continuous RTD activity reaching from
fundamental university studies to world-scale operation and tuning.

Yara is dedicated to continue the development of Fluid Bed granulation technology and is applying a
broad range of competencies in the effort to maintain and further develop the technique.

Key words
Urea, Granulation, Fluid Bed
Approved by Date Signature

Rune Ingels

C:\WINNT\TEMP\C.DOCUME~1.a110174.NH.Notes\4thSnamprogetti1.doc
Postal Address Visiting Address Telephone Telefax Registration No.
Yara International ASA Bygdøy allé 2 +47 24 15 70 00 +47 24 15 70 01 NO 986 228 608 MVA
Post Box 2464 Solli N-0202 Oslo
N-0202 Oslo E-mail
Norway yara@yara.com
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1 Introduction
Granulation technology is often referred to as a practical hands-on dominated
competence. The reason for this is the complexity of this technology, which makes it
difficult to use advanced simulation tools to design or operate the technology.

This is about to change, as the scale of new granulation units is asking for high
reliability and operability, as well as a predictability and accuracy in the design.

This paper is focusing on some key factors for the design and operability of urea
granulation technology.
2 Relevant fundamentals of granulation technologies
Urea production gives one mole of water for each mole of urea, and a 70-72 % solution
is often the standard solution coming from any front-end plant. Evaporation of water is
then clearly both the precursor and an integrated part of the granulation process.
2.1 Heat of formation
A fundamental evaluation of energy required for this starts out with an exothermic
reaction if the process steam can be recovered at 25 o C.

(NH2 )2 CO(aq) + H2O(l) => (NH2 )2CO(s) + H2O(l) ∆H0 = -12 to -13 kJ/mole

If we accept not winning the condensation energy of the evaporated water back, the
calculation will show:

(NH2 )2 CO(aq) + H2O(l) => (NH2 )2CO(s) + H2O(g) ∆H0 = 30-32 kJ/mole

If we as in prilling are also unable to win any of the crystallisation heat back, the
calculation will show:

(NH2 )2 CO(aq) + H2O(l) => (NH2 )2CO(l) + H2O(g) ∆H0 = 41-43 kJ/mole
2.2 Process heat balance
From the heat of formations, the target would be to utilise most of the crystallisation
heat and heat of solution to perform as much as possible of the evaporation in the
granulator.

Given the total heat balance including the sensible heat, heat of solution and heat of
fusion starting from a solution of 125 o C ending with a product out of the granulator of
108 o C, it should be possible to evaporate all the water from an 85 % urea solution.

The practical side of this is not as easy as it sounds. The main challenge in a
granulation process is to grow particles from a sticky solution or mass of urea and
water. The heat and mass transfer rates are limiting factors, and mechanical movement
is required to avoid scaling and provide contact and retention time.

The granulator, being a drum, a pug- mill, fluid drum or a fluid bed requires retention
time for the phase transformation and energy balance to be established and a mechanical
movement to facilitate the particle growth to an acceptable size.
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3 Power consumption granulation and cooling

The main challenge in urea granulation is, as in all granulation processes, to combine
solidification, evaporation/drying and cooling within the physical borderlines given by
the solid liquid system.

Physical handling of urea in the various process steps causes the overall consumption of
electrical energy. Key performance indicators are retention times and recycle ratios.
3.1 Power consumption for lifting in drum or fluid bed granulator
The difference between using fluidised bed or drums in the various steps is not
significant from an energy point of view.

The purpose of a drum as well as a fluidised bed is to create contact between urea
particles and air and/or solution.

In a fluid bed where airflow in the range of 1.5 m/s is required to keep the product
properly fluidised, the required energy consumption can be related to each tonne kept in
the granulator.

1000kg * 9.81m/s2 * 1.6 m/s = approx. 16 kW per tonne in the bed.

Retention time 0.2 h (depending on energy balance)

Loop flow ratio * 1.5 (depend on energy balance and particle balance)
Power efficiency 0.6 (depend on fan and ducting)
*Loop flow is the total flow through the granulator as a factor of the production

This will give 8-9 kWh/tonne of product produced.

A granulation drum can be illustrated in the same way. The rotating drum with its
lifters is used to lift and drop the product through a flow of air. The energy
consumption for this process unit is determined by the same factors as in a fluidised
bed. The lifting speed and the amount of product lifted is determined by the RPM and
the drum design.

Figure 1 is illustrating the lifting principle of a drum.

The drum speed is typically 10 RPM

The average time to lift the product
from bottom to top is 60 s/10 RPM/2 = 3 s
and with an average lifting height of 0.8 D
The lifting velocity for a 4 m drum is
3.2 m/3 sek = 1.07 m/s
1000kg * 9.81 m/s2 * 1.07 m/s = 10 kW per tonne.

Retention time 0.18 h (depending on spraying and lifting principle)

Loop flow ratio 2.7 (depend on energy balance and particle balance)
Power efficiency 0.95
This will give 5 kWh/tonne of product produced.
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The actual design parameters used in the mechanical design of a drum is, however,
showing that the increase of diameter and RPM is increasing the specific energy
consumption. Using a geometrical scale-up of 2:1, keeping RPM and length to diameter
fixed, will give a 26 % increase in specific lifting power (kWh/tonne produced). An
increase in diameter will, however, require an increase in RPM if the contact time
between air and product shall stay kept constant.

Drum designed for up to 2000 MTPD are in most process designs competitive to a
fluidized bed granulator, when the energy for atomisation is not considered.
3.2 Power consumption for loop cooling
Cooling in the granulation is done with:

1) Air through the granulator

2) Air through a fluid bed cooler, only the loop cooler
3) Evaporation of water in the feed solution
4) Heat loss in total loop

Fluid Bed granulation is the only granulation process where cooling in the granulation
unit has a significant effect. The power consumption for the fluidised bed granulator
and atomisation air is relatively high compared to a drum process or for a fluid bed
granulator with high concentration melt. The key indicator for this is the low recycle
ratio. In the Yara fluid bed granulation, the recycle is maintained due to the particle
balance, and not for the cooling of the granulator.

For a classic drum granulation process, the energy balance over the granulator is
maintained through cooling and recycling 2,5 to 3,5 times the product flow.

The cooling duty for this large material flow is performed in the temperature range from
108 o C to 50 o C. With a high ambient temperature, the additional energy for blowing
this cooling air, easily exceed that of the fluid bed granulator. If in addition air
conditioning is required the cost will be very high.

For most European conditions, a drum granulation loop is energy wise fully
competitive, but will loose capacity under summer conditions.

The drum granulation process is also known to give a nice high-density product due the
high concentration melt.

In general terms, the classical drum granulation processes are good alternatives at
capacities around 2000 MTPD, outside extreme ambient conditions.
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Figure 2 is illustrating the basic cooling principles and the connected power
consumption.

(m3/h -> kWh/t)

Scrubber

(m3/h ->kWh/t)

Scrubber
U sol
Air

Air 1
3
(m /h -> kWh/t)
R

Air 2
(m3/h -> kWh/t)

Key issues in Fluid Bed granulation

The fluid bed technology is a typical change from traditional, low intensity techniques,
to high intensity technique, where the scale of equipment or process dimensions is
reduced with a factor of 100,000 or more.

In the nozzle inside the granulator, a combination of evaporation and crystallisation is

taking place. The process takes place in a nozzle of a few cm in diameter, the droplets
are 50 microns, and about 90 % of the process is completed in microseconds.

In prior and alternative technique the evaporation is done in evaporators, crystallisation

in crystallisers or prilling towers, with dimensions of 5-10 meters to the prilling tower
of 60 m.
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3.3 Nozzle
Designing the right type of nozzle is the key to a successful process design. Without the
right nozzle the fluid bed granulation process has lost its competitiveness.

Important design parameters are:

1) Energy and heat balance over the total process

2) Energy and heat balance over the nozzle and in the spraying zone
3) Phase equilibrium, liquid-vapour and liquid-solid in nozzle spray
4) Mass and energy transport between phases
5) Rate of crystallisation, evaporation, super saturation, crystallisation retarding
6) Physical energy utilisation, atomisation and motion in spout
7) Chemical and physical effects additives, biuret, formaldehyde…
8) Product quality, drying and cooling effects, absorption and diffusion rates

Figure 3 is a conceptual illustration of points 2 and 3

PH2O

H2O(g)

Urea Air
solutio
Air
H2O(g)

PH2O

Two of the objectives with a nozzle are to atomise the solution and to evaporate as
much water as possible, without crystallising too much of the urea before the droplet is
hitting a base granule. Warm nozzle air is promoting evaporation and preventing sub-
cooling. Additives are functioning as crystal retardants and final product quality
enhancers. The proof of the optimum process is called accretion, and can be confirmed
by looking at the final granule from the SEM picture.
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Figure 4 is showing the basic principles of particle growth in granulation

CONFIDENTIAL

Granule growth principles

Layering Accretion Agglomeration

RI - Date: 2004 -08 -01 - Page: 26

CONFIDENTIAL

SEM pictures of Yara FB granules

RI - Date: 2004 -08 -01 - Page: 27

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3.4 Spout and particle movement

The nozzle, spout and particle movement are closely connected. It is of outmost
importance that the nozzle is spraying into a moving mass of granules. The nozzle itself
best creates the movement of the granule mass. A relatively large flow of atomising air
is determining the droplet size, the evaporation of water, the sub-cooling and proper
crystallisation ratio for the accretion.

Figure 5 is showing a jet or spout formed in the fluid bed

CONFIDENTIAL

Yara atomiser and particle movement

jet fluidised bed

fluidising air
nozzle
atomisation air
liquid
RI - Date: 2004 -08 -01 - Page: 21

3.5 Bed movement

The nozzle and spout performance is depending on the total bed movement. The energy
and mass dissipation into the bed is critical for total capacity of the process. The nozzle
and spout is a high intensity process, and is not in any way in equilibrium or balance as
an isolated unit.

The bed movement is determined by:

1) The fluidisation air rate

2) The bed height and compartment set- up
3) The spout characteristics
4) Particle size distribution
5) Physical properties of the particles

The close to total mixing pattern, which can easily be measured by colouring some of
the feed particles, seems to be a favourable basic condition. From an operability and
product quality point of view a homogenous temperature profile throughout the bed is
positive. This homogeneity must also be combined with size distribution effects,
segregation and retention time differences to maintain the correct and natural recycle
ratio. Both total mass and number of crushed seed material and undersize recycle are, if
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not designed properly, able to upset the total granulation process and lower the product
quality.
4 Methodology and equipment
Being the owner of a granulation technology like fluid bed, and licensing it to third
parties, implies a significant responsibility in giving guarantees and living up to them.

The basis for guarantees and trust is always a documented and demonstrated ability to
deliver as promised and expected.

Even in, and maybe especially in a large production company like Yara, such
capabilities do not come easily. Our prime objective is to compete with a superior
internal technology and production facilities.

Reference plants and proven technology at world scale, are expensive to use in
troubleshooting or in design or development.
4.1 Pilot plants and modelling
The prime tool in developing a granulation technology is pilot plants. Size and scale up
effects are an everlasting issue, and no philosophy is able to answer to any situation.

Two different philosophies have been practiced in Yara.

The Technology Centre in Porsgrunn has backed up the pilot plant development with
theoretical understanding and modelling or calculation. The required capacity for a
scale-up to industrial scale is then 500-1500 kg/h in capacity, and scale- up to 1000-1500
MTPD is possible. A similar philosophy has been the basis for a successful and long-
lasting business in Kaltenbach-Thuring.

The Technology Centre in Sluiskil has adopted a philosophy of solving and testing most
features in the pilot plants before it is implemented at full scale. The combination of
product development and a dedicated licensing strategy has provided the basis for a
philosophy of going to semi- industrial scale, being 100-140 MTPD as the ultimate
capacity for a pilot plant.

For our fluid bed technology development Yara has adopted the best from both these
philosophies.
4.1.1 Particle movement
Particle movement in the bed, in the spout around the nozzles and in the nozzle itself,
requires several tools and pilot installations. In Sluiskil, two Particle Movement
Characterisation units, PMCs, are available for the most basic testing of ideas and visual
demonstration of certain effects. These units are designed in transparent materials and
operate at ambient conditions.

After an initial idea screening, the purpose of these units is to verify our ability to
predict and model the effects before go ing into larger scale testing. The use of the PMC
and similar units has also successfully been used to develop discrete particle movement
models that are further developed into continuous multiphase models. The next step is
now planned for testing in a commercial CFD simulation tool. This will, if successful,
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provide a powerful tool for simulating more complex geometries and particle growth
mechanisms.

Figure 5, is showing one of the PMC in Sluiskil

Particle Movement
Movement Characterisation

4.1.2 Batch granulator

For the first screening of nozzle performance, a batch unit is used. This unit is operating
at normal process conditions at a scale comparable to a nozzle and a spout. This unit is
able to verify effect of nozzle design. Particle build- up is idealised, but product quality
effects can be verified in this unit.

The batch granulator has a capacity of making a batch 70 kg and is easily operated by
one operator.
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Figure 6, is showing a picture of the batch granulator

Fluid Bed Granulator

Granulator

Hydro Agri
Research
Rob Stevens Centre
Sluiskil

4.1.3 Continuous Research Pilot Plant (RePP) in Sluiskil

A typical size of a research pilot plant operating relatively independent of production
unit is 0.5-1.0 t/h. This is the highest practical capacity before handling the feed and
products become a problem. In such a plant particle growth effects and total mass and
energy balances can be established with the help of some support calculations. Full
scale can easily be done based on full-scale reference data.
4.1.4 Semi Industrial Pilot Plant (SIPP) in Sluiskil
In a plant with a capacity of 100-140 MTPD, all aspects of the process can be tested,
measured and verified. Mass and energy balance, product quality, emissions and
effluent figures and effects can based on SIPP tests be guaranteed.

Equipment design and unit operations can be tested out, and detailed design data
established. Process control, trip systems and process safety can also with a high degree
of certainty be established or verified.

The unit is very practical for test marketing and full scale real testing of product quality
effects through the whole logistical chain. The SIPP is, however, not in use
continuously, as the operating cost of the unit requires good projects to provide a cost
benefit.
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Figure 7, is showing a picture of the granulator in the SIPP

SIPP: GLF501

Hydro Agri
Research
Rob Stevens Centre
Sluiskil

4.1.5 Modelling and simulation

As described in the previous, urea granulation involves different types of competencies
or scientific understanding. More or less advanced calculation methods and modelling
is the difference between the qualitative understanding found in operators and
experience, from the quantitative ability required for designing a full- scale process and
plant.

Process, mass and energy balance

In Hydro, and later Yara, general urea process simulation tools have been developed
since the seventies. The capability of performing a mass and energy balance as well as
rough phase equilibrium for the main components is useful, but not necessary.

A total process simulation is useful when studying recycling effects, and in such cases
the models are often able to verify surprise effects, experienced by operators, but not
understood by the engineers.

Chemistry effects
The phase equilibrium is significantly affected by minor amount of urea derivatives and
additives like formaldehyde.

Modelling of these effects is typically far behind the experience, and calculations and
modelling are limited to generic pH effects in electrolytic systems. Measuring methods
and interpreting results is a not overcome hurdle at present.
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Atomisation and nozzle modelling

Nozzle development has so far been a practical trial and error task, based on general
theory of nozzle and atomisation principles. Applying the system specific physical and
chemical properties has been the key. Today some nozzles can be modelled with
respect to evaporation and crystallisation effects. Applying a standard urea system to a
nozzle process, is confirming 20 years of experience, it is almost impossible!!

5 Yara technology ownership

As described in this paper, urea granulation is both a theoretical and practical challenge.
We have only touched upon a few process design elements. The way from the first
trials made in Sluiskil to the present design is a long chain of trial and error before the
right features are qualified and proven for licensing.

Access to semi industrial-scale and full- scale plants where tests can be made by a
qualified team, is essential for development and troubleshooting. No two plants are
identical. Design specifications are different, because of climate and the client’s
operational frames and objectives.

Yara have licensed its Fluid Bed technology through engineering contractors, and is will
in the future seek to continue this practice. Yara have over the last three years tried to
reset its licensing strategy, and make a distinct difference between what is unrestricted
and what is restricted technologies.

Unrestricted technologies are evaluated for divestment, but restricted technologies will
be developed and used only internally and strategically in J/V and with partners.

5.1 Acknowledgements
This paper is to a large extent based on years of research activities and competence from
RTD environment in Sluiskil and Yara Fertiliser Technology.

I would like to thank Luc Vanmarcke, the RTD Manager in Sluiskil, and Andre
Kayaert, Licensing Manager in HFT, for years of cooperation and their contribution to
this paper.

Rune Ingels
Vice President, Yara International