GB2266712A - Improved prilling process - Google Patents

Improved prilling process Download PDF

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Publication number
GB2266712A
GB2266712A GB9308211A GB9308211A GB2266712A GB 2266712 A GB2266712 A GB 2266712A GB 9308211 A GB9308211 A GB 9308211A GB 9308211 A GB9308211 A GB 9308211A GB 2266712 A GB2266712 A GB 2266712A
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GB
United Kingdom
Prior art keywords
duct
prills
ammonium nitrate
egan
gas flow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
GB9308211A
Other versions
GB9308211D0 (en
GB2266712B (en
Inventor
Raymond Oliver
Ronald Otto Peddie
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
PPG Architectural Coatings Canada Inc
Imperial Chemical Industries Ltd
Original Assignee
ICI Canada Inc
Imperial Chemical Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from GB929209621A external-priority patent/GB9209621D0/en
Application filed by ICI Canada Inc, Imperial Chemical Industries Ltd filed Critical ICI Canada Inc
Priority to GB9308211A priority Critical patent/GB2266712B/en
Priority to TW82103909A priority patent/TW263487B/zh
Publication of GB9308211D0 publication Critical patent/GB9308211D0/en
Publication of GB2266712A publication Critical patent/GB2266712A/en
Application granted granted Critical
Publication of GB2266712B publication Critical patent/GB2266712B/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C1/00Ammonium nitrate fertilisers
    • C05C1/02Granulation; Pelletisation; Stabilisation; Colouring
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B31/00Compositions containing an inorganic nitrogen-oxygen salt
    • C06B31/28Compositions containing an inorganic nitrogen-oxygen salt the salt being ammonium nitrate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Explosive grade ammonium nitrate (EGAN) prills are made by a process that comprises the steps of: a. continuously spraying a 95 to 98% by weight solution/melt of ammonium nitrate (or a mixture of ammonium nitrate and minor proportions of one or more other EGAN - acceptable nitrates) in/with water under spray-head conditions causing the emergent jets to break into cascades of substantially mono-sized droplets; b. allowing the formed droplets to fall within a vertical duct; c. continuously feeding a stream of cooling gas upwards through the duct, the temperature difference of the gas flow between its inlet to the duct and its outlet from the duct being at least 60 DEG C; the falling velocity of the prills being at most 3 metres/second, the upward gas flow velocity being e.g. 6 m/s for 2 mm prill and 9 m/s for 3 mm prill and, optionally, recycling the gas. ade b

Description

IMPROVED PRILL aPROCESS This invention concerns ammonium nitrate prill as used in explosive formulations such as ANFO (which is ammonium nitrate (AN) prill containing absorbed fuel oil (FO) at a level of about 6% by weight or higher) and HANFO, or "Heavy ANFO", which is a blend of AN prill (or ANFO) and emulsion explosive.
Explosives grade ammonium nitrate prill (herein "EGAN" prill) is required to be sufficiently porous to be able to absorb the quantity of fuel oil needed for an effective explosives composition. Porosity, which is indicated comparatively by particle density and bulk density, is affected by the conditions of prill formation (especially the initial water content of the spray melt) and the conditions under which the residual small percentage of water (up to 5% by weight) in the collected product at the base of the prill tower is removed by a drying process (down to e.g. 0.1 to 0.2k by weight). The size of EGAN prill is usually around 2 to 3 mm diameter, but larger diameters are not excluded.
In the specification of copending UK patent application No. 91 24 304.8 a process is described for producing predominantly monosized prills of AN in a prilling tower by a modification of the process described in published EP 0 320 153. The disclosure in UK 91 24 304.8 is as follows:- 111t is known from EP-A-0320153 that the disintegration of a liquid jet comprising a highly concentrated solution of ammonium nitrate can be controlled so as to produce a substantially monosize distribution of droplets and hence, on solidification, particles.The disintegration is controlled by causing the plate, wherein an orifice which produces the liquid jet is located, to vibrate at a predetermined frequency and in a plane substantially perpendicular to the direction of flow of the liquid jet, thereby inducing a so-called asymmetric disturbance on the surface of the liquid jet. The vibration is required to have an amplitude which is substantially smaller than that used in other systems wherein the orifice containing plate is vibrated in a plane parallel to the direction of flow of the liquid jet and/or wherein the orifice containing plate is swung from side to side.The predetermined frequency is required to be calculated according to the expression fopT = Uj. (4.5dj) 1 (1) wherein fopT is the frequency in Hertz, uj is the velocity of the jet from the orifice (m.s -l and dj is the diameter of the orifice (m). The effect of applying a vibration having the predetermined frequency was confirmed using water, which flow properties are similar to those of a highly concentrated solution of ammonium nitrate, and was successfully applied to the prilling of fertilizer grade ammonium nitrate. It is known in the art that fertilizer grade ammonium nitrate is required to have a high bulk density, and to be relatively non-porous.In order to achieve these desired properties the fertilizer grade ammonium nitrate is produced from a highly concentrated ammonium nitrate solution having an ammonium nitrate concentration of at least 99% by weight, which is known in the art as ammonium nitrate melt or molten ammonium nitrate.
Prilling of ammonium nitrate solutions having ammonium nitrate concentrations of less that 99% by weight, e.g. 96% by weight produce a lower density, porous, and physically weaker material which is not as suitable for use as a fertilizer It is also known to use ammonium nitrate as an explosive, however, the required characteristics of explosive grade ammonium nitrate are different from those of fertilizer grade ammonium nitrate in that explosive grade ammonium nitrate is required to be relatively porous so that it is able to more readily absorb the various additives and conditioners used to sensitize it to detonation.Thus, in the preparation of explosive grade ammonium nitrate it is required that a solution having a low concentration of ammonium nitrate, i.e. less than 99% w/w, is prilled and the resulting droplets solidified in a generally similar process to that used for preparation of fertilizer grade ammonium nitrate. In the preparation of explosive grade ammonium nitrate is it also desirable to obtain a monosize distribution of particles. Application of asymmetric vibrations to the orifice containing plate at a predetermined frequency calculated according to the method disclosed in EP-A-0 320 153, however, does not lead to the preparation of explosive grade ammonium nitrate comprising particles having a monosize distribution.
It has now been found that prilling of solutions containing low concentrations of ammonium nitrate can be controlled to give monosize distributions of droplets and hence particles by applying vibrations to be orifice containing plate which are of a frequency determined according to an expression which is different from expression (1).
Accordingly the present invention provides a prilling process wherein a liquid comprising between 90 to 98% w/w ammonium nitrate is caused to flow through an orifice in a plate thereby forming a liquid jet and that as the liquid flows through the orifice the plate is vibrated in a plane substantially perpendicular to the direction of the liquid jet thereby producing a asymmetric disturbance to the surface of the liquid jet and the frequency of the vibration at or within 10% of the optimum frequency as given by the expression:: = u. (7r.205.dj(l + 3z)1 ... (2) fspT = uj .2 5.dj(1 + 3z)-1 ...(2) wherein fopT is the frequency in Hertz, uj is the velocity of the jet from the orifice (m.s-l) , dj is the diameter of the orifice (m), z is the dimensionless group (Wej)=0-5.(Rej)-1, Wej is djuj2p.y 1, Rej is djujp.g-1 p is the density of the liquid (kg.m3), y is the surface tension of the liquid (N.m-l) and g is the viscosity of the liquid (Ns.m One of the differences between the prilling of fertilizer grade ammonium nitrate and explosive grade ammonium nitrate is that the physical properties, in particular the viscosity of the ammonium nitrate solution, influences the hydrodynamics of the droplet formation process thereby preventing the direct use of the expression (1) to determine the optimum frequency of vibration of the orifice containing plate. The viscosity of ammonium nitrate solution is significantly higher than both that of ammonium nitrate melt and also water. Thus, the ammonium nitrate solution is no longer an inviscid liquid, as assumed in derivation of expression (1), but is a viscid liquid the flow properties of which are better described by expression (2). The transition between inviscid and viscid flow is not abrupt.
However, where the viscosity of the liquid is less than 1.5 cP (0.0015 Ns.m~2) then expression (1) is usually more appropriate, whereas at higher viscosities expression (2) is more appropriate.
The plate used in the prilling process is generally circular in plan view and may also be dished such that the liquid jet issues from the convex side of the plate. Generally each plate contains a plurality of orifices, for example from 2000 to 3000 per plate. Although the vibration of the plate may be through a reciprocating translational movement it is particularly convenient to vibrate the plate through a reciprocating rotational movement wherein the axis of rotation is through the plate, e.g. through the centre of the plate, in a direction generally coincident with the direction of the liquid jet or jets produced.
Where the vibration is through a reciprocating rotational movement it is preferred that the vibration has an amplitude equivalent to 10-5 to 10-3 radians of rotation.
The liquid from which explosive grade ammonium nitrate is usually produced comprises a solution containing from 90 to 98% w/w ammonium nitrate, more usually from 92 to 95% w/w ammonium nitrate.
The liquid jet formed by the orifice has a velocity which depends upon the size of the orifice and upon the mass flow rate. The orifice is usually in the form of a circular hole having a diameter from 0.5 to 2 mm, e.g. 0.75, 1.1 or 1.13 mm. In keeping with the teaching of EP-A-0320153 it is also preferred that the flow through the orifice is laminar and uniform flow of the liquid jet is achieved.Similarly, it is preferred that the Reynolds Number does not exceed 2300, and more particularly is in the range from 500 to 2000." We have now found that when conditions are employed at the spray head that cause the creation of substantially mono-sized "melt" droplets (and hence prills) in a mean size within the practical range 1 to 4 mm, usually in the range 2 to 3 mm, as is the case for the process described in UK Application No. 9124304.8, it is possible to effect a beneficial intensification of the prill forming process.
According to this invention EGAN prills are made by a process that comprises the steps of: a. continuously spraying a 95 to 98% by weight (preferably 95% to 96% by weight) solution/melt of ammonium nitrate (or a mixture of ammonium nitrate and minor proportions of one or more other EGAN - acceptable nitrates) in/with water under spray-head conditions causing the emergent jets to break into cascades of substantially mono-sized droplets; b. allowing the formed droplets to fall within a vertical duct; c. continuously feeding a stream of cooling gas (e.g.
ambient air) upwards through the duct to effect cooling and solidification of the falling droplets and some removal of moisture so as to form substantially mono sized EGAN prills of up to about 4 mm diameter, say in the range 2 to 3 mm diameter, and d. continuously withdrawing the EGAN prills collecting at the base of the duct (such EGAN prills then optionally being further cooled and/or dried in a forced draught regime), the process being further characterised by intensification of the upward gas flow regime in the duct such that: (i) the temperature difference of the gas flow between its inlet to the duct and its outlet from the duct is at least about 600C preferably at least about 800 (e.g. up to 20 in and around 1000 out); and (ii) the falling velocity of the prills in the duct is at most about 3, preferably at most about 2, metres/second relative to ground (i.e. a stationary observer external to the duct) the upward gas flow velocity being e.g. 6 m/s relative to ground for 2 mm prill and 9 m/s for 3 mm prill and, optionally, (iii) recycling the gas stream after washing and cooling and addition of any required make-up gas.
Preferably, the upward gas flow regime in the upper level of the duct at the gas outlet from the duct is such that substantially none of the prills is carried out of the duct in the gas stream. This is made possible in the present process by the creation of substantially uniform composition mono-sized droplets below the spray head. The preferred spray head process is that described above with reference to UK Application No. 91 24 304.8.
In the present process the higher gas velocity within the duct (approaching the terminal falling velocity of the prills) leads to a degree of turbulence in the gas flow enhancing prill drying.
The temperature and high evaporative capacity of the effluent gas (e.g. air) at around ambient humidity makes it useful for performing work in the recycle loop e.g. within a wet scrubbing stage.
A significant economic benefit of the present process are the reduction in the required prilling tower dimensions e.g. the diameter reduced to one third or lower and the height reduced to say, two thirds for the same kg/day prill output, and the reduction in gas circulation loading making possible the economic avoidance of gaseous effluent emissions into the atmosphere.
The present process makes available at the base of the duct EGAN prill containing residual moisture at the same sorts of level as the prior referenced process i.e.
preferably 0.1 to 0.5 water by weight. Ordinarily, the ascollected "wet" prill will be further dried in a forced draught regime, conventionally a rotary drum drier.
The melt composition in the present process is preferably an AN/Water melt, aside from any minor inclusions of crystal habit modifiers, anticaking agents and other such property modifiers as already known in the EGAN prior art.
Other nitrates are known as additives to AN in explosives applications and their inclusion in the spray melt as a minor component is therefore not excluded on product grounds. Straight forward tests will establish the compatibility of any desired product ingredient with the intensified prill-forming regime of this invention.

Claims (6)

Claims
1. A process for producing explosive grade ammonium nitrate (EGAN) prills which process comprises the steps of: a. continuously spraying a 95 to 98% by weight solution/melt of ammonium nitrate (or a mixture of ammonium nitrate and minor proportions of one or more other EGAN - acceptable nitrates) in/with water under spray-head conditions causing the emergent jets to break into cascades of substantially mono-sized droplets; b. allowing the formed droplets to fall within a vertical duct; c. continuously feeding a stream of cooling gas (e.g.
ambient air) upwards through the duct to effect cooling and solidification of the falling droplets and some removal of moisture so as to form substantially mono sized EGAN prills of up to about 4 mm diameter, and d. continuously withdrawing the EGAN prills collecting at the base of the duct (such EGAN prills then optionally being further cooled and/or dried in a forced draught regime), the process being further characterised by intensification of the upward gas flow regime in the duct such that: (i) the temperature difference of the gas flow between its inlet to the duct and its outlet from the duct is at least about 600C; and (ii) the falling velocity of the prills in the duct is at most about 3 metres/second relative to ground (i.e. a stationary observer external to the duct) the upward gas flow velocity being e.g 6 m/s relative to ground for 2 mm prill and 9 m/s for 3 mm prill and, optionally, (iii) recycling the gas stream after washing and cooling and addition of any required make-up gas.
2. A process according to claim 1 wherein the upward gas flow regime in the upper level of the duct at the gas outlet from the duct is such that substantially none of the prills is carried out of the duct in the gas stream.
3. A process according to claim 1 or claim 2 wherein the temperature difference of the gas flow between its inlet to the duct and its outlet from the duct is at least about 800C.
4. A process according to any one of claims 1 to 3 wherein the falling velocity of the prills in the duct is at most 2 metres/second relative to ground.
5. A process for producing explosive grade ammonium nitrate prills substantially as hereinbefore described.
6. Explosive grade ammonium nitrate prills whenever produced by a process according to any one of claims 1 to 5.
GB9308211A 1992-05-05 1993-04-21 Improved prilling process Expired - Lifetime GB2266712B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
GB9308211A GB2266712B (en) 1992-05-05 1993-04-21 Improved prilling process
TW82103909A TW263487B (en) 1992-05-05 1993-05-18

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB929209621A GB9209621D0 (en) 1992-05-05 1992-05-05 Improved prill process
GB9308211A GB2266712B (en) 1992-05-05 1993-04-21 Improved prilling process

Publications (3)

Publication Number Publication Date
GB9308211D0 GB9308211D0 (en) 1993-06-02
GB2266712A true GB2266712A (en) 1993-11-10
GB2266712B GB2266712B (en) 1995-12-13

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GB9308211A Expired - Lifetime GB2266712B (en) 1992-05-05 1993-04-21 Improved prilling process

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TW (1) TW263487B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005108296A1 (en) * 2004-05-07 2005-11-17 Yara International Asa Method for producing porous ammonium nitrate

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0320153A1 (en) * 1987-12-07 1989-06-14 Imperial Chemical Industries Plc Controlled break-up of liquid jets

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0320153A1 (en) * 1987-12-07 1989-06-14 Imperial Chemical Industries Plc Controlled break-up of liquid jets

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005108296A1 (en) * 2004-05-07 2005-11-17 Yara International Asa Method for producing porous ammonium nitrate

Also Published As

Publication number Publication date
TW263487B (en) 1995-11-21
GB9308211D0 (en) 1993-06-02
GB2266712B (en) 1995-12-13

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732E Amendments to the register in respect of changes of name or changes affecting rights (sect. 32/1977)
PE20 Patent expired after termination of 20 years

Expiry date: 20130420