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Fertilizer Finishing Process for An
              and NPK’s with Rotoform HS 2000
                                K. SWAMY, U. NANZ, H. KURT
                                  Sandvik Process Systems
                                           Fellbach, Germany

          Innovation has always been the key to success in the fertilizer industry. Better performance
      figures plus a proven track record support these innovations. The key question is how to
      introduce a new technology in situations where it is not yet considered?
          Recent successes in the use of the Rotoform system for sulphur and urea solidification have
      opened up new opportunities in other fertilizer plants. Furthermore, growing demand for higher
      capacity solutions has resulted in the development of the unique Rotoform HS 2000, a system
      that makes use of a 2000 mm wide steel belt to deliver a 33% increase in capacity compared with
      standard Rotoform systems.
          Alongside growth in the use of Rotoform systems for sulphur and urea, Sandvik has also been
      working on the development of Rotoform solutions for new fertilizer products. One such project
      has seen the installation of a mobile Rotoform unit at the site of Romanian fertilizer producer
      Azomures, and pilot tests have resulted in the successful development of a number new products
      and applications, including Ammonium Nitrate (AN) and AN-based NPK fertilizers, both pure and
      in mixtures.
          As a result, Azomures decided to invest in two Rotoform HS 2000 lines for its AN and NPK
      modernization project; these two units were delivered in July 2011 and commissioning is
      scheduled for completion by the end of 2011.

INTRODUCTION
1.      Existing AN & NPK facilities in Azomures
The existing Stamicarbon-design plant at Azomures SA’s facility in Tirgu Mures, Romania was installed in
1972. It is an ammonium nitrate (AN) 33.5% / calcium ammonium nitrate (CAN) 27% plant with a design
capacity of 1400 mtpd AN and 1600 mtpd CAN.

                                                  - 325 -
K.Swamy, U. Nanz, H. Kurt


Some 750 mtpd of the AN solution is produced as a byproduct of the N-H Odda process Nitrophosphate NPK
plant and the rest is a product of three plants applying direct neutralization of nitric acid and ammonia. The AN
solution from the Nitrophosphate plant (at 82 wt%) – together with synthetically produced AN – is pre-
concentrated to 95 wt% and then pumped to a granulation plant. The third neutralization plant still operates
with a prilling tower.
The following plants were considered for the revamping project:
Ammonium Nitrate 1+2
•         Up to 625 mtpd AN produced by neutralization
•         Up to 750 mtpd AN produced as by-product from NPK plant
•         Total 1,400 mtpd granulation unit at downstream
Ammonium Nitrate 3
•         Up to 800 mtpd AN produced by neutralization
•         Solidification by prilling
NPK Plant
•         Two lines, each neutralizing up to 165 mtpd 100% P2O5
•         Physical capacity limits around 1,300 mtpd per line
•         Both lines have solidification by prilling
2.        Need for modernization and alternatives evaluated
The aim of the management team at Azomures was to replace the AN/CAN prills with a product of a higher
quality, one that would better meet the needs of international markets and therefore attract a higher prices.
The following finishing technologies were compared and evaluated:
1.        Prilling tower
2.        Granulation technology
3.        Sandvik Rotoform
Prilling and granulation are the most common processes used to produce solid ammonium nitrate.
PRILLING
To produce prills, concentrated melt is sprayed into the top of a prill tower. In the tower, ammonium nitrate
droplets fall countercurrent to a rising air stream that cools and solidifies the falling droplets into spherical
prills. Prill density can be varied by using different concentrations of ammonium nitrate melt.
GRANULATION
Various granulation technologies are available to produce solid ammonium nitrate: high solid recycle
processes like rotary drum & pug mill and low solid recycle processes like pan & fluid bed granulation
technology.
High recycle processes have a typical recycle of 1.5-2 while the low recycle processes stay below a recycle
rate of 1. These differences result in different AN concentrations or amount of liquid phase required by the
granulation process. A high solid recycle granulation usually requires a lower AN concentration (94-96.5%)
than a low solid recycle process (98-99.5%). This correspondingly means that the amount of water to be
removed from the product by drying is higher for a high recycle process. Some low recycle processes operate
with such a low water content so that a dryer is not required.
Common parts of granulation processes are obviously the granulator, where the granules are formed from
smaller parts (seeds). Granules are removed from the granulator and screened. Offsize granules are crushed
and recycled to the granulator to supply additional seed particles or are dissolved and returned to the solution
process.

326                                          Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
Fertilizer finishing process for AN & NPKs with Rotoform HS 2000


 The temperature of the ammonium nitrate product exiting the solids formation process is approximately 66 to
 124°C. Rotary drum or fluidized bed cooling prevents deterioration and agglomeration of solids before storage
 and shipping.
 Since the solids are produced in a wide variety of sizes, they must be screened for consistently sized prills or
 granules. Cooled prills are screened and offsize prills are dissolved and recycled to the solution concentration
 process. Granules are screened before cooling. Undersize particles are returned directly to the granulator and
 oversize granules may be either crushed and returned to the granulator or sent to the solution concentration
 process.
 Emissions from the prilling tower and granulation sections are ammonium nitrate dust and ammonia.
 Emissions from prill towers result from carryover of fine particles and fumes by the cooling air flowing through
 the tower. These fine particles are from microprill formation, created by prills colliding with the tower or with
 one another, and from rapid transition of the ammonia nitrate between crystal states. The uncontrolled dust
 emissions from prill towers are therefore affected by tower airflow, spray melt temperature, condition and type
 of melt spray device, air temperature, and crystal state changes of the solid prills.
 The amount of microprill mass that can be entrained in the prill tower exhaust is determined by the tower air
 velocity. Increasing spray melt temperature causes an increase in the amount of gas-phase ammonium nitrate
 generated. Thus, gaseous emissions from high density prilling (1.59 g dust per kg AN without scrubber, 0.6
 g/kg AN with a wet dust scrubber) are greater than from low density ammonium prilling towers (0.46 g/kg AN
 without scrubber, 0.26 g/kg with a wet dust scrubber).
 The granulation process in general provides a larger degree of control in product formation than does prilling.
 Granulation produces a solid ammonium nitrate product that, relative to prills, is larger and has greater
 abrasion resistance and crushing strength. The air flow in granulation processes is lower than that in prilling
 operations. The design and operating parameters of granulators may affect emission rates. Cooling and drying
 are usually conducted in rotary drums, fluid bed or bulk flow coolers. As with granulators, the design and
 operating parameters of the rotary drums, fluid bed and bulk flow coolers may affect the quantity of emissions.
 In addition to design parameters, prill and granule temperature control is necessary to control emissions from
 disintegration of solids caused by changes in crystal state.
 Emissions from screening operations are generated by the attrition of the ammonium nitrate solids against the
 screens and against one another. Almost all screening operations used in the ammonium nitrate
 manufacturing industry are enclosed or have a cover over the uppermost screen. Rotary drum granulators
 have a typical dust emission of 0.22 g dust per kg produced ammonium nitrate when applying a wet dust
 scrubber.
 SANDVIK ROTOFORM®
 The Sandvik Rotoform system cools and crystallizes the ammonium nitrate melt indirectly with cooling water.
 The lack of any need for air flow in order to remove the heat delivers two key benefits. Firstly, as the
 ammonium nitrate can be solidified without the need for large air blowers, energy consumption is significantly
 lower, and secondly, there is no need to manage large air flows loaded with ammonium nitrate dust.
 Another advantage of the Sandvik Rotoform is the production of a solid product with a very narrow size
 distribution. No screening, crushing or large recycle streams are involved, eliminating the investment costs
 associated with this equipment.
 Following is an overview of various features of the different finishing technologies used to produce solid
 ammonium nitrate.




Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)                          327
K.Swamy, U. Nanz, H. Kurt


                                                      Table 1
                                 Comparison of prilling, granulation and Rotoform
        Product                  Prilling                            Granulation                            Rotoform

      Product size   1.5-2.0 mm                           3.0-4.0 mm                            1.5-4.0 mm
      (mm)
      Control of     Relatively wide size                 Partial control via choice of         Narrow distribution, can be
      size/size      distribution; partial control        screens, however typically            controlled by exchanging
      distribution   possible by adjusting prilling       large recycle flows, key              Rotoform rotating shell.
                     bucket design and rpm                elements are nozzle and
                                                          residence time
      Production     Difficult                            Limited                               Easy and many possibilities
      of specialty
      products
      Control of     Difficult                            Feasible                              Easy and variable
      discharge
      temp.
      Capacity       500 (minimum)                        500 (minimum)                         150 (based on product size);
      (mtpd)                                                                                    several lines can be installed
                                                                                                in parallel enabling flexibility
                                                                                                to cope with varying
                                                                                                throughput. No upscale risks.
      Cooling        Large airflow                        Significant amount of air             No air, indirect water cooling
      media                                               depending on granulation
                                                          technology
      L.P. Steam     Low                                  Higher                                Low
      consumption
      Electrical     Moderate for forced draft            High                                  Low
      consumption    prilling towers
      Dust           Yes, amount depends on               Yes, amount depends on                No dust generation
      generation     plant load and ambient               plant load and ambient
                     condition                            condition (but <prilling due to
                                                          extra dust scrubber)
      Equipment      Scraper cleaning (monthly)           Monthly or flushing after             Monthly or flushing after
      washing                                             stoppage (cleaning takes 8            stoppage (cleaning takes 3
                                                          hours)                                hours); One spare line for
                                                                                                several units means no
                                                                                                stoppage necessary.
      Ease of        Easy                                 Less easy, cleaning required          Easy operation with minimum
      operation                                                                                 equipment


Azomures chose for the Sandvik Rotoform system for the following key reasons:
    to minimize the emission of dust and free-ammonia from the prilling plants
    to produce more higher value, specialty fertilizer products

The following options are currently under evaluation:
1.       Install Sandvik Rotoform lines plus a mixing unit at AN 3 plant and shut down the current prilling tower


328                                                   Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
Fertilizer finishing process for AN & NPKs with Rotoform HS 2000


 2.         Install Sandvik Rotoform lines plus a mixing unit at NPK plant and shut down the existing two prilling
            towers
 3.         Analyze feasibility of installing Sandvik Rotoform lines plus a mixing unit for independent production of
            greenhouse grade calcium nitrate

 3.      Chosen finishing technology: Sandvik Rotoform HS 2000
 The figure below shows the flow scheme of the Rotoform technology.




                                              Fig 1: Sandvik Rotoform pastillation process
 The feed to the Rotoform is ammonium nitrate melt at a concentration of 99.8 wt%; in existing AN plants this
 feed can be branched off from the ammonium nitrate evaporation section downstream of the ammonium
 nitrate melt pumps.
 Ammonium nitrate melt is introduced under pressure
 (2-3 bar) to the dropformer. The Rotoform HS (High
 Speed) 2000 dropformer, patented by Sandvik,
 consists of a heated stator and a perforated rotating
 shell that turns concentrically around the stator to
 deposit drops of ammonium nitrate across the full
 width of the 2000 mm wide steel belt.
 The circumferential speed of the Rotoformer is
 synchronized with the speed of the steel belt
 ensuring that the drops are deposited on the belt
 without deformation and, after solidification, results in
 regular pastilles with an optimum shape.                  Fig 2: Rotating shell delivers droplets of the required size




Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)                               329
K.Swamy, U. Nanz, H. Kurt




                            Picture 1: Ammonium nitrate pastilles on the steel cooling belt
The rotating shell contains rows of small holes which are sized to deliver the melt onto the belt in the required
product size. As the belt travels along the system, cooling water sprayed against the underside of the belt
absorbs the heat released from the melt – and transferred via the steel belt – during crystallization and cooling.
The water is collected in pans, cooled in a cooling system (cooling tower) and reused over and over again.
As well as enabling continual recycling of cooling water, this indirect cooling method also means there is
absolutely no risk or cross-contamination between product and cooling medium; the cooling water cannot
come into contact with the ammonium nitrate, and vice versa.
ACCURATE TEMPERATURE CONTROL
It is well known that ammonium nitrate (33.5 %) has a critical temperature at 32.2 oC. At this temperature, the
crystalline structure of ammonium nitrate is rhombic system 4, which changes to rhombic system 3 if the
temperature exceeds this temperature. In addition, it will change to tetragonal system 5 if the temperature falls
below -16.8 oC. These changes in crystalline structure lead to disintegration of the product after a few cycles
around these temperatures and increase the tendency to caking.
                                                    Table 2
                                   Crystal structures of Ammonium Nitrate

                System      Temperature (°C)                    State                 Volume change (%)

                    -             >169.6                        liquid                          -
                    I         169.6 to 125.2                    cubic                         +2.1
                   II          125.2 to 84.2                  tetragonal                       -1.3
                   III         84.2 to 32.3                   α-rhombic                       +3.6
                   IV          32.3 to −16.8                  β-rhombic                       −2.9
                   V              −16.8                       tetragonal                        -
The Sandvik Rotoform enables efficient and extremely accurate control of product temperature by the simple
means of setting the right cooling water temperatures at the cooling belt areas.




330                                              Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
Fertilizer finishing process for AN & NPKs with Rotoform HS 2000




                                           Fig 3: Precise temperature control with Rotoform
 After solidification, the pastilles are released smoothly from the steel belt via an oscillating scraper. The
 product then falls directly onto a conveyor belt for transfer to storage. The section above the moving steel belt
 is enclosed with a hood and vented to an existing vent system.
 There are no large air flows involved in this technology and there is no visible ammonium nitrate dust
 emission. Should ammonia vapours be produced, these can be easily captured in a simple atmospheric
 absorber; this results in negligible emissions of ammonia and dust, a unique feature of this technology.




        Picture 2: Rotoform skid mounted equipment showing the hood that captures any ammonia and dust emissions


Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)                              331
K.Swamy, U. Nanz, H. Kurt




                             Picture 3: Front view of installation of four Rotoform units.
The size of the Rotoform product is same as for granules, and can be easily varied between 1.5 and 4.0 mm.
The pastilles are extremely uniform, even more so than granules. It goes without saying that the Rotoform
product quality is significant better than prills; experience has shown that farmers who have applied the
pastilles were very satisfied and prepared to pay a premium price compared with prills.




                                     Picture 4: Farmers prefer pastilles to prills
Using Rotoform solidification, with a typical capacity of some 125-150 mtpd, it is possible to produce all kinds
of specialty ammonium nitrate and NPK products. The following products have been all been produced on
Rotoform systems:
•       Fertilizer grade urea
•       Technical urea for urea-formaldehyde, melamine, ad blue production
•       Urea blended with macro nutrients
•       Urea blended with micro nutrients
•       Urea with ammonium sulphate
•       Ammonium nitrate
•       Ammonium nitrate derivatives (KCl, Zeolite, AS < 10% and NPK)
•       NPK complex fertilizer from nitrate & ammonium nitrate route
•       Calcium nitrate based on special melts prepared by customers
•       Magnesium nitrate
•       Sulphur bentonite
•       Sulphur bentonite and zinc
Following is a reference list of Rotoform technology used for fertilizer products


332                                            Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
Fertilizer finishing process for AN & NPKs with Rotoform HS 2000



                                                 Table 4: Rotoform reference list

                                                 Company/
           Year          Plant capacity                                 Status              Product/application
                                                 location

                                                 KEMIRA /                                   Urea + phosphates /
           2000          1 Flaker                                       Operational
                                                 Dubai                                      Fertilizer

                         1 Rotoform              ESSECO /                                   Sulphur bentonite /
           2000                                                         Operational
                         120 mtpd                Italy                                      Fertilizer

                         1 Rotoform              Coogee /                                   Sulphur bentonite /
           2002                                                         Operational
                         120 mtpd                Australia                                  Fertilizer

                         1 Pilot unit,           PCS /                                      Fertilizer urea /
           2004                                                         Operational
                         Rotoform                Tennessee, USA                             technical urea

                         1 Rotoform              Coromandel /                               Sulphur bentonite /
           2005                                                         Operational
                         120 mtpd                India                                      Fertilizer

                         PLANT                   COMPANY/
           YEAR                                                         STATUS              PRODUCT/APPLICATION
                         CAPACITY                LOCATION

                         5 Rotoforms             PCS /
           2006                                                         Operational         Technical grade urea
                         300 mtpd                Georgia, USA

           2006
                         4 Rotoforms             Zlotniki /                                 Mg-N + CaN
           till                                                         Operational
                         240 mtpd                Poland                                     / Fertilizer
           2009

                         Pilot production
                                                 YARA. / Brunsb.                            Urea +10%S /
           2008          unit                                           Pilot
                                                 Germany                                    Fertilizer urea
                         125 mtpd

                                                 ACRON / Velikiy
                         1 Rotoform                                                         Technical and
           2008                                  Novgorod /             Operational
                         120 mtpd                                                           fertilizer urea
                                                 Russia

                         1 Pilot Rotoform
                                                 Petrobras                                  Urea + additives /
           2010          + dosing, mixing                               Pre commissioning
                                                 Sergipe / Brazil                           Urea based fertilizers
                         & grinding

                         Rotoform +
                         mixing and              Azomures                                   AN with ingredients /
           2010                                                         Commissioning
                         grinding 200            Romania                                    Fertilizer
                         mtpd

                         Rotoform +
                         dosing, mixing &        Azomures                                   NPK with ingredients /
           2010                                                         Commissioning
                         grinding 200            Romania                                    Fertilizer
                         mtpd

                         2 Rotoforms
                                                 SABIC
           2011          240 mtpd + down                                Installation        Technical grade urea
                                                 Al Bayroni / KSA
                         stream

Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)                                333
K.Swamy, U. Nanz, H. Kurt


The production process of these specialty fertilizer products is fairly simple and straightforward. In some cases
one simply injects a liquid additive in the melt, in others a blending unit is applied to grind and mix the solid
additives in the melt.
For example, for urea plus ammonium sulphate, urea melt and solid AS are mixed and ground in two steps in
a blending unit (a standard packaged unit). Up to 40% wt. AS has been mixed with urea with excellent results.




                                      Fig 3: Flow scheme to produce urea+AS




                                    Picture 5: Blending unit to produce urea/AS
The introduction of specialty ammonium nitrate products can be achieved smoothly and easily, requiring just a
single Rotoform line which can be brought into and out of production whenever required. When market
demand increases, additional lines can be installed in parallel. The pictures below show various specialty
products.


334                                           Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
Fertilizer finishing process for AN & NPKs with Rotoform HS 2000




                                             Picture 6: Various Rotoform fertilizer products
 4.        Validation tests
 The finishing sections traditionally used in the production of ammonium nitrate and ammonium nitrate based
 fertilizer products – i.e. prilling towers and granulation sections –typically have minimum capacity of 500 to
 1000 mtpd. With the Sandvik Rotoform, the capacity of a single line is about 150 mtpd. However, as multiple
 lines can be installed in parallel, it is possible to achieve much higher capacities and – importantly – vary
 production in response to market demand.
 Although the performance and reliability of Rotoform was proven and recognized in relation to sulphur and
 urea processing, no Rotoform line had previously been installed for pure ammonium nitrate or ammonium
 nitrate based NPKs.
 Understandably, Azomures therefore wanted to undertake a validation process to ensure that the company’s
 investment in Rotoform was the right one, and that the exact process and operational data for each product
 would be readily available at the full scale commercial start up.
 Moreover the production of different mixtures of ammonium nitrate and ammonium nitrate-based NPKs during
 validation tests would provide a series of special fertilizer products, with which market testing could be carried
 out. By doing so, Azomures was able to streamline long term marketing strategy during the implementation of
 commercial scale project.
 Over the course of few weeks, Azomures will be able to validate the following products:
        Ammonium sulphate/nitrate – by feeding solid ammonium sulphate to the ammonium nitrate melt
        Urea/ammonium nitrate – by using AN and urea melts
        Non-detonating grade AN – by feeding anti-detonation agent to AN melt
        CAN – by feeding dolomite to AN melt
        NK 21-0-21 – by feeding MOP to AN melt
        Higher K2O containing NPK fertilizers – by adding higher quantities MOP to AN melt
        Flexibly to produce other more exotic NPK formulations – by adding higher quantities of P2O5 as MAP
           and/or K2O as MOP
 5.        Project details and status
 After the successful validation tests on a pilot scale Rotoform line, Azomures decided to install two commercial
 scale Sandvik Rotoform HS 2000 lines.
 Delivery time for the two Sandvik Rotoform HS 2000 lines was only eight months. Six weeks were needed to
 install the two Rotoform lines and over the next three months Azomures would produce several batches of
 different products on these units.



Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)                           335
K.Swamy, U. Nanz, H. Kurt


After six months, Azomures would decide to install an additional 17 Rotoformer HS 2000 lines to convert its
total product capacity into Sandvik Rotoform. The delivery time for two trains of six Rotoformer HS 2000 lines –
each with a mixing unit – was only nine months. The final train of Rotoform HS 2000 lines with mixing unit will
be delivered in twelve months.
By October 2011 the two Rotoformer lines had been delivered and installed at Azomures. The commissioning
phase has been started and commercial production is expected in March 2012.
6.       Benefits to Azomures of Sandvik Rotoform solution
The installation of Sandvik Rotoform as finishing technology for Azomures’ ammonium nitrate plant will bring
the following benefits:
      Ability to produce specially customized, premium quality fertilizer products
      Flexibility in production in order to meet market demand for each of these products
      Ability to undertake market introduction and field trials in parallel with implementation of commercial
         scale capacity
      Significant reduction in emission figures
      Easy operation and maintenance due to small footprint
      100% availability through the use of parallel extra line
References:
1.Revamping of an AN/CAN prilling plant to produce a granular product of high quality, Pan and Dimitri Orphanides,
      Orphanides Consultants, Greece, 2000 IFA Technical Symposium, New Orleans, USA
2.Inorganic Chemical Industry, Ammonium Nitrate (7/93), p. 8.3-1 to 8.3-9
3.Guidance for the storage, handling and transportation of solid mineral materials, EFMA, April 2007
4.The Uhde Pugmill Granulation, the process for safe and reliable production of CAN and other AN based Fertilizers, Peter
      Kamermann, 2006 IFA Technical Symposium, Vilnius, Lithuania




336                                               Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)

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Sandvik process systems kumar swamy (paper)

  • 1. Fertilizer Finishing Process for An and NPK’s with Rotoform HS 2000 K. SWAMY, U. NANZ, H. KURT Sandvik Process Systems Fellbach, Germany Innovation has always been the key to success in the fertilizer industry. Better performance figures plus a proven track record support these innovations. The key question is how to introduce a new technology in situations where it is not yet considered? Recent successes in the use of the Rotoform system for sulphur and urea solidification have opened up new opportunities in other fertilizer plants. Furthermore, growing demand for higher capacity solutions has resulted in the development of the unique Rotoform HS 2000, a system that makes use of a 2000 mm wide steel belt to deliver a 33% increase in capacity compared with standard Rotoform systems. Alongside growth in the use of Rotoform systems for sulphur and urea, Sandvik has also been working on the development of Rotoform solutions for new fertilizer products. One such project has seen the installation of a mobile Rotoform unit at the site of Romanian fertilizer producer Azomures, and pilot tests have resulted in the successful development of a number new products and applications, including Ammonium Nitrate (AN) and AN-based NPK fertilizers, both pure and in mixtures. As a result, Azomures decided to invest in two Rotoform HS 2000 lines for its AN and NPK modernization project; these two units were delivered in July 2011 and commissioning is scheduled for completion by the end of 2011. INTRODUCTION 1. Existing AN & NPK facilities in Azomures The existing Stamicarbon-design plant at Azomures SA’s facility in Tirgu Mures, Romania was installed in 1972. It is an ammonium nitrate (AN) 33.5% / calcium ammonium nitrate (CAN) 27% plant with a design capacity of 1400 mtpd AN and 1600 mtpd CAN. - 325 -
  • 2. K.Swamy, U. Nanz, H. Kurt Some 750 mtpd of the AN solution is produced as a byproduct of the N-H Odda process Nitrophosphate NPK plant and the rest is a product of three plants applying direct neutralization of nitric acid and ammonia. The AN solution from the Nitrophosphate plant (at 82 wt%) – together with synthetically produced AN – is pre- concentrated to 95 wt% and then pumped to a granulation plant. The third neutralization plant still operates with a prilling tower. The following plants were considered for the revamping project: Ammonium Nitrate 1+2 • Up to 625 mtpd AN produced by neutralization • Up to 750 mtpd AN produced as by-product from NPK plant • Total 1,400 mtpd granulation unit at downstream Ammonium Nitrate 3 • Up to 800 mtpd AN produced by neutralization • Solidification by prilling NPK Plant • Two lines, each neutralizing up to 165 mtpd 100% P2O5 • Physical capacity limits around 1,300 mtpd per line • Both lines have solidification by prilling 2. Need for modernization and alternatives evaluated The aim of the management team at Azomures was to replace the AN/CAN prills with a product of a higher quality, one that would better meet the needs of international markets and therefore attract a higher prices. The following finishing technologies were compared and evaluated: 1. Prilling tower 2. Granulation technology 3. Sandvik Rotoform Prilling and granulation are the most common processes used to produce solid ammonium nitrate. PRILLING To produce prills, concentrated melt is sprayed into the top of a prill tower. In the tower, ammonium nitrate droplets fall countercurrent to a rising air stream that cools and solidifies the falling droplets into spherical prills. Prill density can be varied by using different concentrations of ammonium nitrate melt. GRANULATION Various granulation technologies are available to produce solid ammonium nitrate: high solid recycle processes like rotary drum & pug mill and low solid recycle processes like pan & fluid bed granulation technology. High recycle processes have a typical recycle of 1.5-2 while the low recycle processes stay below a recycle rate of 1. These differences result in different AN concentrations or amount of liquid phase required by the granulation process. A high solid recycle granulation usually requires a lower AN concentration (94-96.5%) than a low solid recycle process (98-99.5%). This correspondingly means that the amount of water to be removed from the product by drying is higher for a high recycle process. Some low recycle processes operate with such a low water content so that a dryer is not required. Common parts of granulation processes are obviously the granulator, where the granules are formed from smaller parts (seeds). Granules are removed from the granulator and screened. Offsize granules are crushed and recycled to the granulator to supply additional seed particles or are dissolved and returned to the solution process. 326 Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
  • 3. Fertilizer finishing process for AN & NPKs with Rotoform HS 2000 The temperature of the ammonium nitrate product exiting the solids formation process is approximately 66 to 124°C. Rotary drum or fluidized bed cooling prevents deterioration and agglomeration of solids before storage and shipping. Since the solids are produced in a wide variety of sizes, they must be screened for consistently sized prills or granules. Cooled prills are screened and offsize prills are dissolved and recycled to the solution concentration process. Granules are screened before cooling. Undersize particles are returned directly to the granulator and oversize granules may be either crushed and returned to the granulator or sent to the solution concentration process. Emissions from the prilling tower and granulation sections are ammonium nitrate dust and ammonia. Emissions from prill towers result from carryover of fine particles and fumes by the cooling air flowing through the tower. These fine particles are from microprill formation, created by prills colliding with the tower or with one another, and from rapid transition of the ammonia nitrate between crystal states. The uncontrolled dust emissions from prill towers are therefore affected by tower airflow, spray melt temperature, condition and type of melt spray device, air temperature, and crystal state changes of the solid prills. The amount of microprill mass that can be entrained in the prill tower exhaust is determined by the tower air velocity. Increasing spray melt temperature causes an increase in the amount of gas-phase ammonium nitrate generated. Thus, gaseous emissions from high density prilling (1.59 g dust per kg AN without scrubber, 0.6 g/kg AN with a wet dust scrubber) are greater than from low density ammonium prilling towers (0.46 g/kg AN without scrubber, 0.26 g/kg with a wet dust scrubber). The granulation process in general provides a larger degree of control in product formation than does prilling. Granulation produces a solid ammonium nitrate product that, relative to prills, is larger and has greater abrasion resistance and crushing strength. The air flow in granulation processes is lower than that in prilling operations. The design and operating parameters of granulators may affect emission rates. Cooling and drying are usually conducted in rotary drums, fluid bed or bulk flow coolers. As with granulators, the design and operating parameters of the rotary drums, fluid bed and bulk flow coolers may affect the quantity of emissions. In addition to design parameters, prill and granule temperature control is necessary to control emissions from disintegration of solids caused by changes in crystal state. Emissions from screening operations are generated by the attrition of the ammonium nitrate solids against the screens and against one another. Almost all screening operations used in the ammonium nitrate manufacturing industry are enclosed or have a cover over the uppermost screen. Rotary drum granulators have a typical dust emission of 0.22 g dust per kg produced ammonium nitrate when applying a wet dust scrubber. SANDVIK ROTOFORM® The Sandvik Rotoform system cools and crystallizes the ammonium nitrate melt indirectly with cooling water. The lack of any need for air flow in order to remove the heat delivers two key benefits. Firstly, as the ammonium nitrate can be solidified without the need for large air blowers, energy consumption is significantly lower, and secondly, there is no need to manage large air flows loaded with ammonium nitrate dust. Another advantage of the Sandvik Rotoform is the production of a solid product with a very narrow size distribution. No screening, crushing or large recycle streams are involved, eliminating the investment costs associated with this equipment. Following is an overview of various features of the different finishing technologies used to produce solid ammonium nitrate. Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012) 327
  • 4. K.Swamy, U. Nanz, H. Kurt Table 1 Comparison of prilling, granulation and Rotoform Product Prilling Granulation Rotoform Product size 1.5-2.0 mm 3.0-4.0 mm 1.5-4.0 mm (mm) Control of Relatively wide size Partial control via choice of Narrow distribution, can be size/size distribution; partial control screens, however typically controlled by exchanging distribution possible by adjusting prilling large recycle flows, key Rotoform rotating shell. bucket design and rpm elements are nozzle and residence time Production Difficult Limited Easy and many possibilities of specialty products Control of Difficult Feasible Easy and variable discharge temp. Capacity 500 (minimum) 500 (minimum) 150 (based on product size); (mtpd) several lines can be installed in parallel enabling flexibility to cope with varying throughput. No upscale risks. Cooling Large airflow Significant amount of air No air, indirect water cooling media depending on granulation technology L.P. Steam Low Higher Low consumption Electrical Moderate for forced draft High Low consumption prilling towers Dust Yes, amount depends on Yes, amount depends on No dust generation generation plant load and ambient plant load and ambient condition condition (but <prilling due to extra dust scrubber) Equipment Scraper cleaning (monthly) Monthly or flushing after Monthly or flushing after washing stoppage (cleaning takes 8 stoppage (cleaning takes 3 hours) hours); One spare line for several units means no stoppage necessary. Ease of Easy Less easy, cleaning required Easy operation with minimum operation equipment Azomures chose for the Sandvik Rotoform system for the following key reasons:  to minimize the emission of dust and free-ammonia from the prilling plants  to produce more higher value, specialty fertilizer products The following options are currently under evaluation: 1. Install Sandvik Rotoform lines plus a mixing unit at AN 3 plant and shut down the current prilling tower 328 Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
  • 5. Fertilizer finishing process for AN & NPKs with Rotoform HS 2000 2. Install Sandvik Rotoform lines plus a mixing unit at NPK plant and shut down the existing two prilling towers 3. Analyze feasibility of installing Sandvik Rotoform lines plus a mixing unit for independent production of greenhouse grade calcium nitrate 3. Chosen finishing technology: Sandvik Rotoform HS 2000 The figure below shows the flow scheme of the Rotoform technology. Fig 1: Sandvik Rotoform pastillation process The feed to the Rotoform is ammonium nitrate melt at a concentration of 99.8 wt%; in existing AN plants this feed can be branched off from the ammonium nitrate evaporation section downstream of the ammonium nitrate melt pumps. Ammonium nitrate melt is introduced under pressure (2-3 bar) to the dropformer. The Rotoform HS (High Speed) 2000 dropformer, patented by Sandvik, consists of a heated stator and a perforated rotating shell that turns concentrically around the stator to deposit drops of ammonium nitrate across the full width of the 2000 mm wide steel belt. The circumferential speed of the Rotoformer is synchronized with the speed of the steel belt ensuring that the drops are deposited on the belt without deformation and, after solidification, results in regular pastilles with an optimum shape. Fig 2: Rotating shell delivers droplets of the required size Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012) 329
  • 6. K.Swamy, U. Nanz, H. Kurt Picture 1: Ammonium nitrate pastilles on the steel cooling belt The rotating shell contains rows of small holes which are sized to deliver the melt onto the belt in the required product size. As the belt travels along the system, cooling water sprayed against the underside of the belt absorbs the heat released from the melt – and transferred via the steel belt – during crystallization and cooling. The water is collected in pans, cooled in a cooling system (cooling tower) and reused over and over again. As well as enabling continual recycling of cooling water, this indirect cooling method also means there is absolutely no risk or cross-contamination between product and cooling medium; the cooling water cannot come into contact with the ammonium nitrate, and vice versa. ACCURATE TEMPERATURE CONTROL It is well known that ammonium nitrate (33.5 %) has a critical temperature at 32.2 oC. At this temperature, the crystalline structure of ammonium nitrate is rhombic system 4, which changes to rhombic system 3 if the temperature exceeds this temperature. In addition, it will change to tetragonal system 5 if the temperature falls below -16.8 oC. These changes in crystalline structure lead to disintegration of the product after a few cycles around these temperatures and increase the tendency to caking. Table 2 Crystal structures of Ammonium Nitrate System Temperature (°C) State Volume change (%) - >169.6 liquid - I 169.6 to 125.2 cubic +2.1 II 125.2 to 84.2 tetragonal -1.3 III 84.2 to 32.3 α-rhombic +3.6 IV 32.3 to −16.8 β-rhombic −2.9 V −16.8 tetragonal - The Sandvik Rotoform enables efficient and extremely accurate control of product temperature by the simple means of setting the right cooling water temperatures at the cooling belt areas. 330 Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
  • 7. Fertilizer finishing process for AN & NPKs with Rotoform HS 2000 Fig 3: Precise temperature control with Rotoform After solidification, the pastilles are released smoothly from the steel belt via an oscillating scraper. The product then falls directly onto a conveyor belt for transfer to storage. The section above the moving steel belt is enclosed with a hood and vented to an existing vent system. There are no large air flows involved in this technology and there is no visible ammonium nitrate dust emission. Should ammonia vapours be produced, these can be easily captured in a simple atmospheric absorber; this results in negligible emissions of ammonia and dust, a unique feature of this technology. Picture 2: Rotoform skid mounted equipment showing the hood that captures any ammonia and dust emissions Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012) 331
  • 8. K.Swamy, U. Nanz, H. Kurt Picture 3: Front view of installation of four Rotoform units. The size of the Rotoform product is same as for granules, and can be easily varied between 1.5 and 4.0 mm. The pastilles are extremely uniform, even more so than granules. It goes without saying that the Rotoform product quality is significant better than prills; experience has shown that farmers who have applied the pastilles were very satisfied and prepared to pay a premium price compared with prills. Picture 4: Farmers prefer pastilles to prills Using Rotoform solidification, with a typical capacity of some 125-150 mtpd, it is possible to produce all kinds of specialty ammonium nitrate and NPK products. The following products have been all been produced on Rotoform systems: • Fertilizer grade urea • Technical urea for urea-formaldehyde, melamine, ad blue production • Urea blended with macro nutrients • Urea blended with micro nutrients • Urea with ammonium sulphate • Ammonium nitrate • Ammonium nitrate derivatives (KCl, Zeolite, AS < 10% and NPK) • NPK complex fertilizer from nitrate & ammonium nitrate route • Calcium nitrate based on special melts prepared by customers • Magnesium nitrate • Sulphur bentonite • Sulphur bentonite and zinc Following is a reference list of Rotoform technology used for fertilizer products 332 Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
  • 9. Fertilizer finishing process for AN & NPKs with Rotoform HS 2000 Table 4: Rotoform reference list Company/ Year Plant capacity Status Product/application location KEMIRA / Urea + phosphates / 2000 1 Flaker Operational Dubai Fertilizer 1 Rotoform ESSECO / Sulphur bentonite / 2000 Operational 120 mtpd Italy Fertilizer 1 Rotoform Coogee / Sulphur bentonite / 2002 Operational 120 mtpd Australia Fertilizer 1 Pilot unit, PCS / Fertilizer urea / 2004 Operational Rotoform Tennessee, USA technical urea 1 Rotoform Coromandel / Sulphur bentonite / 2005 Operational 120 mtpd India Fertilizer PLANT COMPANY/ YEAR STATUS PRODUCT/APPLICATION CAPACITY LOCATION 5 Rotoforms PCS / 2006 Operational Technical grade urea 300 mtpd Georgia, USA 2006 4 Rotoforms Zlotniki / Mg-N + CaN till Operational 240 mtpd Poland / Fertilizer 2009 Pilot production YARA. / Brunsb. Urea +10%S / 2008 unit Pilot Germany Fertilizer urea 125 mtpd ACRON / Velikiy 1 Rotoform Technical and 2008 Novgorod / Operational 120 mtpd fertilizer urea Russia 1 Pilot Rotoform Petrobras Urea + additives / 2010 + dosing, mixing Pre commissioning Sergipe / Brazil Urea based fertilizers & grinding Rotoform + mixing and Azomures AN with ingredients / 2010 Commissioning grinding 200 Romania Fertilizer mtpd Rotoform + dosing, mixing & Azomures NPK with ingredients / 2010 Commissioning grinding 200 Romania Fertilizer mtpd 2 Rotoforms SABIC 2011 240 mtpd + down Installation Technical grade urea Al Bayroni / KSA stream Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012) 333
  • 10. K.Swamy, U. Nanz, H. Kurt The production process of these specialty fertilizer products is fairly simple and straightforward. In some cases one simply injects a liquid additive in the melt, in others a blending unit is applied to grind and mix the solid additives in the melt. For example, for urea plus ammonium sulphate, urea melt and solid AS are mixed and ground in two steps in a blending unit (a standard packaged unit). Up to 40% wt. AS has been mixed with urea with excellent results. Fig 3: Flow scheme to produce urea+AS Picture 5: Blending unit to produce urea/AS The introduction of specialty ammonium nitrate products can be achieved smoothly and easily, requiring just a single Rotoform line which can be brought into and out of production whenever required. When market demand increases, additional lines can be installed in parallel. The pictures below show various specialty products. 334 Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)
  • 11. Fertilizer finishing process for AN & NPKs with Rotoform HS 2000 Picture 6: Various Rotoform fertilizer products 4. Validation tests The finishing sections traditionally used in the production of ammonium nitrate and ammonium nitrate based fertilizer products – i.e. prilling towers and granulation sections –typically have minimum capacity of 500 to 1000 mtpd. With the Sandvik Rotoform, the capacity of a single line is about 150 mtpd. However, as multiple lines can be installed in parallel, it is possible to achieve much higher capacities and – importantly – vary production in response to market demand. Although the performance and reliability of Rotoform was proven and recognized in relation to sulphur and urea processing, no Rotoform line had previously been installed for pure ammonium nitrate or ammonium nitrate based NPKs. Understandably, Azomures therefore wanted to undertake a validation process to ensure that the company’s investment in Rotoform was the right one, and that the exact process and operational data for each product would be readily available at the full scale commercial start up. Moreover the production of different mixtures of ammonium nitrate and ammonium nitrate-based NPKs during validation tests would provide a series of special fertilizer products, with which market testing could be carried out. By doing so, Azomures was able to streamline long term marketing strategy during the implementation of commercial scale project. Over the course of few weeks, Azomures will be able to validate the following products:  Ammonium sulphate/nitrate – by feeding solid ammonium sulphate to the ammonium nitrate melt  Urea/ammonium nitrate – by using AN and urea melts  Non-detonating grade AN – by feeding anti-detonation agent to AN melt  CAN – by feeding dolomite to AN melt  NK 21-0-21 – by feeding MOP to AN melt  Higher K2O containing NPK fertilizers – by adding higher quantities MOP to AN melt  Flexibly to produce other more exotic NPK formulations – by adding higher quantities of P2O5 as MAP and/or K2O as MOP 5. Project details and status After the successful validation tests on a pilot scale Rotoform line, Azomures decided to install two commercial scale Sandvik Rotoform HS 2000 lines. Delivery time for the two Sandvik Rotoform HS 2000 lines was only eight months. Six weeks were needed to install the two Rotoform lines and over the next three months Azomures would produce several batches of different products on these units. Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012) 335
  • 12. K.Swamy, U. Nanz, H. Kurt After six months, Azomures would decide to install an additional 17 Rotoformer HS 2000 lines to convert its total product capacity into Sandvik Rotoform. The delivery time for two trains of six Rotoformer HS 2000 lines – each with a mixing unit – was only nine months. The final train of Rotoform HS 2000 lines with mixing unit will be delivered in twelve months. By October 2011 the two Rotoformer lines had been delivered and installed at Azomures. The commissioning phase has been started and commercial production is expected in March 2012. 6. Benefits to Azomures of Sandvik Rotoform solution The installation of Sandvik Rotoform as finishing technology for Azomures’ ammonium nitrate plant will bring the following benefits:  Ability to produce specially customized, premium quality fertilizer products  Flexibility in production in order to meet market demand for each of these products  Ability to undertake market introduction and field trials in parallel with implementation of commercial scale capacity  Significant reduction in emission figures  Easy operation and maintenance due to small footprint  100% availability through the use of parallel extra line References: 1.Revamping of an AN/CAN prilling plant to produce a granular product of high quality, Pan and Dimitri Orphanides, Orphanides Consultants, Greece, 2000 IFA Technical Symposium, New Orleans, USA 2.Inorganic Chemical Industry, Ammonium Nitrate (7/93), p. 8.3-1 to 8.3-9 3.Guidance for the storage, handling and transportation of solid mineral materials, EFMA, April 2007 4.The Uhde Pugmill Granulation, the process for safe and reliable production of CAN and other AN based Fertilizers, Peter Kamermann, 2006 IFA Technical Symposium, Vilnius, Lithuania 336 Nitrogen + Syngas 2012 International Conference (Athens, Greece, 20-23 February 2012)