DOI 10.

1007/s10556-016-0090-z
Chemical and Petroleum Engineering, Vol. 51, Nos. 910, January, 2016 (Russian Original Nos. 910, Sept.Oct., 2015)

RESEARCH, DESIGN, CALCULATIONS,

AND OPERATING EXPERIENCE
PROCESSES AND EQUIPMENT FOR CHEMICAL
AND OIL-GAS PRODUCTION

REVAMPING EQUIPMENT AND TECHNOLOGY

OF EXISTING GRANULATING PLANTS TO IMPROVE
THE QUALITY OF GRANULATED PRODUCTS

Yu. A. Taran and A. L. Taran

Finish granulation and encapsulation by fattening technology are used as additional stages to existing
granule production process (for example, by prilling technology). The proposed procedure for calculating
the dynamics of granule size distribution of the supplied external recycle that is processed into the final
product can be applied in the cases of random change in granule growth rate, which allows one to take
into account, among others, abrasion of granules, operation in granulation mode and at the final stage of
granule abrasion (polishing), and nonuniformity of atomization of the applied product and several other
technological procedures and process characteristics.
Keywords: granulation, ammonium nitrate, urea, disk granulators.

The process of layer-by-layer application of the original product on the surface of granules of an external recycle by
pelletizing technology is called fattening [13]. The applied constituents (melt, solution, suspension, emulsion, powder, etc.)
are used with or without a binder and the apparatuses are of drum, disk, and other types [15]. This technology is used for im-
parting the required properties to the surface before encapsulation , strengthening granules, introducing the needed additives,
creating multilayered granules with controlled release of components, enlarging granule size, and other purposes [1, 4]. In all
cases, it is important to know the dynamics of change in granule size distribution. The static strength of the granules and their
resistance to heating cooling thermal cycles [during enantiotropic (reversible, kind I) polymorphic transformations in the
crystalline phase] depend on the composition, physicochemical properties, and state of the applied substance as well as on
the composition and quantity of the proposed additives [2, 3].
Disk granulators can be used to get higher-quality coating and to ensure practically recycle-free process, thanks to
the segregating effect of the disk [13]. As an example, let us consider the possibility of readjustment of the existing plants
for producing nitrogen-containing mineral fertilizers by prilling (in granulation towers) and by minimal (often without inter-
rupting operation of the plant) revamping of the functioning units (production of ammonium nitrate, urea, NPK fertilizers,
etc.) for easily adjustable manufacture of a broad range of higher-quality products.
By revamping the units for production of prilled ammonium nitrate (or creation of stand-alone mobile plants), ammoni-
um nitrate with fillers and porous ammonium nitrate (PAN) can be produced. The fillers are copper, dolomite, limestone (CAN),

Moscow State University of Fine Chemical Technology (MITKhT), Moscow, Russia; e-mail: capsula2@mail.ru. Translated from Khimicheskoe
i Neftegazovoe Mashinostroenie, No. 9, pp. 38, September, 2015.

0009-2355/16/0910-0581 2016 Springer Science+Business Media New York 581

 Fig. 1. Flowchart of finish granulation plant: 1) storage for powdery fillers, additive components, and
microcomponents; 2) hoppers and batchers of powdery additive components; 3, 4) hoppers and batchers
of fillers and microcomponents; 5) unit for preparing binder solution with additives; 6) disk granulator
block; 7) unit for conditioning, applying microcomponents, growth substances, and storing; 8) unit for
storing and supplying microcomponents and growth substances; 9) unit for storing and supplying con-
ditioning agent; I) prilled granules from tower; II) fertilizer solution before evaporation (for NH4NO3
from ITN apparatus 92.5%, for urea 70% before evaporation or 93% after the first stage of evaporation).

ammonium sulfate (NS), potassium-containing component NK, phosphorus-containing component NP, etc. In producing ammo-
nium nitrate with fillers, ammonia consumption per ton of the finished product decreases by at least 0.1 ton compared to ammoni-
um nitrate alone, other consumption coefficients also decrease, thus reducing the product cost. Economic gain accrues also from
the production of PAN the price of PAN is at least 15% higher than the price of prilled agricultural ammonium nitrate.
Products having increased static granule strength and resistance to heating cooling thermal cycles (20 60C)
and PAN incorporated with microporous fillers and protective components are required.
At present, the quality requirements for the finished product (size increase, improvement of granule size distribution, in-
crease in static strength, etc.) are being toughened. For example, according to the recommendation of the European Commission
[Commission of the European Communities, Brussels, 14.09.2001/02 12(COD), Vol. 1, Regulation of the European Parliament
and the Council relating to fertilizers, Annex I List of types of EC fertilizers], the finished product CAN (calcium-ammoni-
um nitrate) must meet the following technical specifications: total nitrate and ammonium nitrogen content in dry substance
2628 wt.%, water content not more than 2 wt.%, Ca and Mg content on CaCO3 basis not more than 20 wt.%; granule size
distribution: 35 mm fraction not less than 96%; static granule strength 26 N/granule (2600 g/granule); friability 100%.
Such a product cannot be obtained by granulation of filler-impregnated ammonium nitrate melt suspension in granu-
lating towers. When drum apparatuses are used for granulation, the recycle ratio reaches 3, in which case the granule surface
quality deteriorates, making the product pulverulent and increasing its clumping tendency. In one of the plants, we put into
operation a pilot plant (PP) for producing up to 80,000 tons/year of calcium-ammonium nitrate by fattening technology. This
technology can be employed to produce ammonium nitrate with a variety of fillers. The experience at hand can be used to
reduce development and designing time.
In organizing production (by continuous three-shift operation) of up to 200,000 tons/year of granulated ammonium
nitrate with fillers or PAN in an ammonium nitrate producing unit, provision was made that, after the renovation carried out
without shutdown of the main plant, the possibility of simultaneous production of conventional ammonium nitrate persists.
The above-noted products are obtained by finish granulation (fattening) of prilled ammonium nitrate with a powdery (fine-
grained) filler using 8090% solution or melt of ammonium nitrate modified by the proposed additives as a binder.
The research and R&D work carried out demonstrated that a product superior in all respects to the specifications
of the EC Commission can be obtained by the proposed technology at a low temperature of 50C using a simple and safe
process flowchart. In this case, conversion of Ca- and Mg-containing filler is practically ruled out.

582
 Air to
For irrigation atmosphere
Air
cleaning SP from
Preparation of aqueous
Cross-linking Emulsifying Tank Batching neutralization
Batching solution of emulsifying
additive storage additive storage
additive

Pore-forming Preparation of solution Tank Standpipe.

Batching
additive storage of pore-forming additive Mixing of
solution with
Batching pore-forming
MgO additive
storage NH4NO3 melt, 99.7% Granu-
Batching lation Air from
Mixing with melt atmosphere
Batching
Cooling in
Melt
cryog. system Air from
pumping atmosphere
Heated
air
Circulation HNO3 Pneumatic NH4NO3 Screening
Preparation of Evaporation solution, 90%
of weak transport (heated)
AKV solution
NH4NO3
solutions
Additive Additive Mixer Surfactant
Storage of ground dolomite, treatment
Filter Binder
limestone, converted chalk solution
(for production of ASN
Liquid ammonium sulfate nitrate or Packing
additives Final neutralization another base component of filler) Nozzle and storing
Heating Unloading
HNO3 Feed hopper Batcher Feeder Disk
Neutralization granulator
Pulp vapor NH3 Filler receiving
hopper
To scrubber

Fig. 2. Flowchart of revamped ammonium nitrate plant in AS-72 unit for production of ammonium nitrate with
fillers and PAN (the revamped blocks are marked by dashed lines).

The pilot-scale tests were conducted in a unit (Fig. 1) consisting of four disk granulators (diameter 2 m, output up to
7 tons/h). The technology can be implemented successfully both in nitrogen fertilizer plants (by adding to the existing units)
and in stand-alone facilities (near ammonium nitrate storages), as was done in the PP.
The prilled saltpeter granules are collected past the tower or from the storage at the ambient temperature in the quan-
tity needed for material balance (worked out for each finished form) and supplied as recycle to a system of paired disk granu-
lators. The ground fillers (particle size not larger than 200 m) are fed at ambient temperature into the paired disk granulators
through batchers and feeders. Simultaneously, the binding solution (melt) of ammonium nitrate with the proposed additives
is sprayed by hot air into the same granulators through pneumatic nozzles. The binding solution is prepared in a separate con-
tainer, into which is injected a complex additive (for cementing the filler powder on the original granule and for bounding the
water in the finished product). The finished granules sized 33.5 mm (without drying, sieving, and re-entry of recycle) with
temperatures up to 45C proceed to the transporter and then for treatment with anticlumping agents, packing (for example, in
big-bags), and storage. In producing PAN from prilled ammonium nitrate (GOST 285), the fraction passing through a 2-mm
sieve is sifted out and used as the external recycle, the fillers are microporous and protective powders (PAN can be obtained
without fillers). The disk granulators are provided with hoppers and a system of gravity batchers for ammonium nitrate gran-
ules and filler powder. The air from the disk granulators is cleaned in bag or irrigated felt filters or by a functioning technology
(discharged into an existing system of gas purifying units of ammonium nitrate plant [2, 3]) and then let off to the atmosphere
with a dust content of 30 mg/m3.

583
 Revamping of the plant (Fig. 2) includes construction of a filler powder receiving hopper, a system of filler batch-
ing and delivery to disk granulators, a hopper for receiving ammonium nitrate granules from the tower, a system of storage,
delivery, and batching of modifying additives (caustic magnesite, ammonium sulfate, etc.) into a tank for preparing binder
solution, a system of delivery and batching of granulated ammonium nitrate into disk granulators, a system for transporting
saltpeter, filler, and finished product granules, a system of tanks for preparing binder solution (8090% ammonium nitrate
solution from ITN apparatus), disk granulators with a piping system, a system for cooling granular product and its treatment
with anticlumping agents (if needed), a finished product packing unit, a bag filter for cleaning dust discharges from the disk
granulators (or another system of filtration of dust-laden air), and a system of automation and control and measuring instru-
ments (CMI). In this case, it is essential to develop new algorithms and revamp the technological process control system.
Approximate capital investments for building a plant. The total expenditures for building a plant with a capacity
of up to 200,000 tons/yr for finish granulation of prilled ammonium nitrate will be 1.44 mln , which includes expenditures
of 0.6 mln for domestic equipment and materials, 0.3 mln for imported equipment, 0.3 mln for construction and
installation work, 0.12 mln for initial data development and associated design, and 0.12 mln for technological project
preparation and know-how.
The expenditures cited are based on calculation for the product of the new equipment (without transportation cost).
The expenditures can be reduced if the plant has the needed equipment. Expenditures for building a stand-alone unit are
at least 40% higher. Expenditures depend essentially on the existence of the needed infrastructure and cost of building the
needed infrastructure components. The approximate time of payback of all expenditures for revamping is not more than
six months (without taking account of higher price for better quality product obtained by fattening technology compared to
prilled product).
Calculation of particle-size distribution of obtained product. The material balance equation with respect to the
end component for batch or continuous (transitional, unsteady) granulation process is [4]:

(1)

where Gg, Ggp, Ggs are, respectively, the mass flow rate of the initial granules, granulated product, and finish-granulating
powder suspension, kg/h; am is the concentration of the finish-granulating mixture; = Ggsam /Gg is the degree of finish
granulation of the original recycle; M = Ggpt is the mass of all components in the apparatus, kg; and t is the average time of
granule residence in the apparatus, h.
The change in current mass M(m) for granules with a mass m in the apparatus in time :

(2)

where Mg(m) = GgFg(m) is the mass flow rate of granules with a mass from 0 to m entering the apparatus with the original
recycle; Fg(m) is the original recycle granule mass distribution function; Mgp(m) = GgpFgp(m) is the mass flow rate of gran-
ules with a mass from 0 to m left from the apparatus with finish-granulated recycle (with the product); Fgp(m) is the product
granule mass distribution function at the outlet;

is the mass flow rate of increment of mass of granules with a mass from 0 to m due to their increase upon finish granulation
with a dimensionless rate of increase of granule mass; sec1; dF(m)/dm = (m) is the current distribution

density of mass m of product granules at the finish granulation entrance; is the mass flow rate
of granules whose mass became larger than m and they expelled from the space the masses 0m; and dF(m)/dm = (m) is the
sought distribution density of the mass m of the product granules in the course of finish granulation.

584
 After putting the cited correlations in Eq. (2), we get:

(3)

or

(4)

Let us transform (4):

(5)

From Eq. (5), we get the equation for calculating the dynamic change in mass distribution as the process passes to
standard conditions:

(6)

where = Ggp /Gg is the degree of finish granulation.

Equation (6) can be solved numerically:

(7)

where is the difference analog of the first derivative: m = mjJ.

In the steady case (after passing to continuous process) at dM/d = 0 or at a low finish granulation rate (for example,
encapsulation, dM/d 0), we get from (1) Gg(1 + ) = Ggp and Fgp(m) = F(m).
In that case, since dF(m)/d = 0, the granule distribution by mass (and, consequently, by size) ceases to change with
time, and Eq. (5) takes the form:

(8)

(9)

585
in finite differences

(10)

For the whole distribution range (0 < m < ), Fg(m) 1, F(m) 1, dF(m)/dm 0; we will then get from (9):

(11)

The difference analog of Eq. (11):

(12)

For approximate estimations, we can get from Eq. (12) the correlation between and t, confining ourselves to a

single term of the sum

(13)

Equations (9) and (11) or their difference analogs (10) and (12) (for ease of use of (13)) should be solved jointly.
From Eq. (9) or (10), we get the density distribution (m) and from Eq. (11) or (12) (for ease of use of (13)), the correlation
between t and , and if it does not coincide with the set correlation, we shall determine more accurately the density distribu-
tion (m) by iteration until convergence of the set correlation between t and .
Let us differentiate Eq. (9) with respect to m to calculate the density distribution at the moment of transition of the
finish granulation process to steady distribution by mass:

(14)

Equation (14) can be solved numerically:

(15)

The dimensionless granule mass growth rate is

It was shown earlier [2, 6] that in the case of finish granulation with a powder, it can be assumed that the linear
growth rate vl = dr/d = const, whence
dm1/3 dr
K = K = const,
d d
where K and K are constants that can be obtained by the expression for the correlation of mass growth rate v(m) via the linear
growth rate vl.
Then,
(16)

586
 Fig. 3. Ammonium nitrate granule density distribution by size upon finish
granulation by rolling (linear granule growth rate vl = 4105 m/sec): 1) initial
distribution as per GOST 285; 2) final distribution (time 1 h, degree of finish
granulation 40%); 3, 4) transitional process (time 20 and 40 min, respectively).

Putting (16) in (14), we get:

(17)

For numerical solution of Eq. (17), use can be made of the difference analog

(18)

and from the equation of balance over the whole distribution (12), 0 m , by putting (18) in it, we get:

(19)

Equation (19) can be solved numerically using its difference analog:

(20)

Equations (17) and (19) must be solved jointly. At a fixed degree of finish granulation and average time of residence
in the apparatus, we get from (17) the product mass density distribution by granule mass (m) and from (19), the correlation
between and t, which can be determined more precisely by iteration.
The problem in (17)(19) has an analytical solution [5]. To solve, the problem must be presented in the form:

(21)

(22)

where = m/m0 is the divergence of the current mass from the average mass; is the ratio of the inverse value
of the average dimensionless granule mass growth rate to the average residence time.

587
 Fig. 4. Size-wise granule distribution density calculated by various methods
(linear granule growth rate vl = 4105 m/sec): 1) initial distribution as per
GOST 285; 2) final distribution by Eq. (24); 3) final distribution for process
time 1 h by Eq. (15) with due regard for Eq. (12).

The solution of the problem in (21)(22) by quadratures has the form [4]:

(23)

or in finite differences:

(24)

where = Jj.
The described problems are solved using difference analogs of Eqs. (5) or (6), (9), (11), (13), and (17)(19). The
proposed procedure for calculating the dynamics of granule size distribution of the supplied external recycle processed into
the end product is applicable for cases of random change in granule growth rate, which allows one to take account of abrasion
of granules, operation under conditions of granulation and (in the final stage) of abrasion (polishing) of granules, and to take
account of the nonuniformity of dispersion of the applied product and of a few other technological procedures and process
characteristics. The calculation results for transition of the process to the steady state are plotted in Fig. 3.
The results of earlier calculation by [4] and our numerical calculations are plotted in Fig. 4 for a comparison. Deter-
mination of the granule growth rate vl put in (16) was discussed in [2, 5]. The heat transfer process in fattening technology in
apparatuses for applying coatings by rolling (in the case of finish granulation [5] and encapsulation ) was studied in [6, 7].
As shown in [2], fattening technology ensures improved static strength of treated granules (especially of prills
obtained in towers) and, in most cases, resistance to heatingcooling thermal cycles in the neighborhood of equilibrium tem-
perature of reversible polymorphic transformation. The additives (modifiers of class I and II) introduced into the finish granu-
lating solution (melt), their treatment (activation), technology of their introduction into finish granulating solution (melt), and
application of the solution (melt) on the granule surface [2, 3, 8, 9] produce a decisive effect. The primary defect of prills is
the presence of shrink channel on the granule surface [2, 3, 10]. Finish granulation [2, 4] makes the granule surface defect-free
and also suitable for high-quality encapsulation by thin (16 vol.%) polymer films. Fattening technology can be applied for
producing multicomponent granules (including from chemically interacting substances) [1, 2, 8, 9].

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588
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