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Chemical and Petroleum Engineering, Vol. 47, Nos. 56, September, 2011 (Russian Original Nos.

56, MayJune, 2011)


I. G. Grishaev and A. M. Norov

A calculation procedure is developed for the productivity of a drum granulator and dryer (DGD) in ammonium phosphate production. It is shown that it determines the permissible heat carrier moisture content and ammonia content within it. These parameters are connected through the original phosphoric acid concentration. A dependence is observed experimentally under industrial conditions for product consolidation on ammonification time in a tubular reactor. A mechanism is proposed for lamellar granule formation, affecting ammonium phosphate quality. Drying regimes and granulation are recommended, minimizing the lammelar granule content of the product.

Granulated ammonium phosphate is used extensively as a mineral fertilizer, for whose production a scheme is used with an ammonizer-granulator (AG) and a drying drum (DD) [1]. Units operating by this technology are highly productive (5060 tons/h) and are universal, i.e., they are suitable for producing a broad range of fertilizers. A disadvantage of the AG and DD scheme is the considerable metal content, and the recycled volume of exhausted gases, cleaning requirements, also sticking of product in drainage pipes between the equipment, and the shift in the amount of commercial product in the direction of coarsening, which makes it impossible to manufacture product with different grain size compositions (for example, 25 and 14 mm) without changing the regime and structural parameters of the layout. Disadvantages of the AG and DD layout are overcome with a combination of drying and granulation in one piece of equipment, i.e., a drum granulator and drier (DGD). This layout is more compact, it consumes less gas, it is amenable to cleaning and external recycling. Spraying and partial dewatering of the pulp in an accompanying stream of heat carrier excludes formation of coarse granules and growths in the equipment, as a result of which a more uniform product grain size composition is achieved. DGD are often used successfully for manufacturing ammonium phosphate [2]. The productivity of one production system (5060 tons/h) is limited by the moisture content and consumption of exhausted drying agent (EDA). In the production of diammonium phosphate (DAP), a limiting parameter in addition is the content of ammonia in EDA. Its equilibrium pressure over DAP is greater than over ammonium phosphate, and therefore during drying of heat carrier it contains a significant amount of free ammonia. The concentration of moisture and ammonia in EDA governs the moisture content and chemical composition of the product, and the consumption of heat carrier governs productivity with a prescribed temperature regime. Ammonia in DAP is neutralized in an absorption assembly by wet-process phosphoric acid (WPA). In order to close the cycle, it is necessary that the amount of WPA provides absorption of this ammonia. Conformity of the amount of moisture and ammonia in EDA is achieved by selecting the WPA concentration. Moisture removal, breakthrough of ammonia from a DGD, and the proportional consumption of it by WPA, i.e., productivity, are interconnected through heat carrier flow rate. The flow rate of EDA and the required (equilibrium with discharged product) content of ammonia within it, determines the absolute amount of ammonia entering into the absorption assembly. Ammonization of WPA in this assembly from the point of view of maintaining pulp fluidity is carried out up to a molar ration (MR) NH3:H3PO4 = 0.4. Whence the consumption of P2O5 considered and the productivity with respect to finSamoilov Research Institute for Fertilizers and Insectofungicides (NIUIF), Moscow, Russia. Translated from Khimicheskoe i Neftegazovoe Mashinostroenie, No. 5, pp. 2223, May, 2011. 324 0009-2355/11/0506-0324 2011 Springer Science+Business Media, Inc.

Fig. 1. Dependence of lamellar granule content in product la on pulp dwell time in tubular reactor tu.

ished product are worked out. In some cases, for example, with a reduction in the amount of dust in EDA or a reduction of the impurity content in WPA, ammonization in absorption may be carried out up to MR > 0.4. However, the order of calculating productivity is unchanged, and the excess part of WPA is fed to a high-speed ammonizer and evaporator (HAE). The permissible concentration of WPA is determined as the ratio of P2O5 consumption to the sum of consumption of 100% WPA corresponding to it, water, evaporated in the DGD as a result of burning natural gas and the heat of ammonization in a tubular reactor (TR), and also water, evaporated in the prior neutralization equipment, for example, in the HAE. The amount of moisture evaporated in the DGD and HAE in terms of ammonia consumption may be connected with air consumption (Gair). Then the concentration of acid, entering into ammonization in the production of DAP, CWPA = 36% P2O5. For the ammonium phosphate production, CWPA = 42% P2O5. A reduction in the concentration of acid leads to a reduction in productivity, and an increase of it increases viscosity of the absorption liquid and DAP pulp, which worsens granule formation conditions in the DGD and operation of the gas cleaning assembly. Drawing attention to the requirement of using water in fertilizer technology for irrigating the second stages of absorption, the concentration of WPA at the inlet to the workshop, according to industrial data, should be greater by 11.5% (abs.). Taking account of the permissible moisture content (according to industrial data) of EDA for DAP (d2 = 0.25 kg/kg air) the content of ammonia in it (GNH3 = 0.036 kg/kg air), the degree of ammonization of WPA in the absorber ((MR = 4) P2O5 consumption may be expressed in terms of air consumption: GP2O5 = 0.375Gair. Productivity with respect to DAP GDAP = 0.815Gair. For ammonium phosphate, drawing attention to satisfactory pulp fluidity with a moisture content of 20%, productivity GAP = Gair. The productivity of a DGD 4.5 m in diameter with respect to DAP is 49 tons/h, and for ammonium phosphate it is 61 tons/h. These are rough values since all coefficients are calculated with some reserve, connected with the possibility of short periods of time and high productivity. On the other hand, for operation of industrial equipment the effect of a multitude of factors is not always considered, which may lead to a reduction in productivity. Deviations also arise with a change in specifications for product quality. One of these factors with a steady-state thermal regime is periodic changes in the charge grain size composition (refinement coarsening), and also connected with the weight of the layer and density of curtains of falling material in the DGD [3]. Moreover, with an increase in the content of fine fractions, caking of the product is strengthened [4]. During mixing of acid and ammonia, there is chemical reaction with formation of supersaturated solution of new substance. Part of this substance in accordance with its temperature and solubility is precipitated in the form of crystals. Previously for the production of ammonium phosphate drying of pulp with a moisture content of 2835% has been recommended [2]. In this case for forming the majority of crystals the dwell time in the reactor operating at atmospheric pressure 325

is sufficient. However, as seen from the results of calculations performed above, a tendency towards an increase in productivity leads to a requirement for use of concentrated pulp and reactors under pressure. Dewatering of pulp during constriction (at the outlet from the TR) and drying leads to formation of new crystals and growth of existing ones. These crystals either form independent particles (nuclei), or coalesce with other particles, i.e., either there is an increase in the content of fine fractions in a charge, or growth of granules. With insufficient dwell time of substance in the liquid phase, which is typical for ammonization of WPA in a TR and intense dewatering in thin films on the recycling surface or within the free volume of a DGD, crystallization is sharply retarded. The formed granules consist of fine crystals and thickened solution. The more of the latter, then the greater the number of lamellar granules. Previously the effect has been established of these, in particular fine, granules on caking [5]. In order to reduce the amount of lamellar granules, it is necessary to provide formation of a considerable part of crystals before moisture removal. Consequently, an important role in creating the structure of a substance is played by the ammonization method. Studies in industrial equipment (TR diameter 0.4 m, DGD 4.5 m in diameter) with a productivity of 3035 tons/h, established that the amount of lamellar granules in a product depends on the dwell time in the TR. As may be seen from the curve (Fig. 1), with an increase in holding time for pulp between ammonization and atomization in the DGD from 16 to 106 sec the average content of lamellar granules falls from 12.5 to 2%. Growth of this index at 137 sec may be explained by cooling of the pulp in an uninsulated pipeline, which initiates formation of an additional amount of fine crystals. Consequently, in holding pulp in a pipeline after TR for 50100 sec the product contains 23% of lamellar granules, which is entirely permissible. Minimization of caking is achieved by increasing the dwell time in the TR, which promotes crystal growth; with an increase in solubility and a reduction in viscosity due to maintenance of a high pulp temperature (heating of atomized agent), which slows down charge refinement; with a reduction in the specific irrigation of recirculated pulp by increasing of atomizing and maintaining a constant of external recycling; with an increase in drying time. Stabilization of recycling flow rate and heating of atomizing agent also promotes smoothing of oscillations in the grain size composition of a charge, which reduces the probability of forming fine lamellar granules, i.e., it reduces product caking. Thus, with observation of the optimum ammonization, drying and granulation regimes the procedure proposed makes it possible by prescribing heat carrier flow rate, to determine the concentration of the original WPA, productivity with respect to product of the required quality, and to calculate the material balance with a closed cycle with respect to ammonia.

REFERENCES 1. 2. 3. 4. 5. I. G. Grishaev and V. A. Grinevich, Study of granulation in a tubular reactor ammonizer granulator unit, Khim. Prom. Segod., No. 8, 812 (2006). I. G. Grishaev and A. A. Brodskii, Treatment of ammonium phosphate pulp with a different moisture content in industrial drum granulators and driers, Khim. Prom., No. 5, 3436 (2002). I. G. Grishaev, Granule formation in a gasliquid stream, submerged in a stream of descending material, Khim. Prom., No. 11, 720724 (1999). V. V. Davydenko, A. M. Norov, I. G. Frishaev, et al., Experience of technical re-equipment of production for ammonium phosphate fertilizer, in: Mir Sery, N, P and K, NIUIF, Moscow, (2011), Iss. 2, pp. 35. I. G. Grishaev, A. Ya. Syrchenkov, and Z. A. Tikhonovich, Regimes for forming lamellar ammonium phosphate granules, Khim. Prom. Segod., No. 1, 2022 (2004).