WO2013043099A2 - Procédé pour fabriquer des particules et particules fabriquées ainsi - Google Patents

Procédé pour fabriquer des particules et particules fabriquées ainsi Download PDF

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Publication number
WO2013043099A2
WO2013043099A2 PCT/SE2012/000139 SE2012000139W WO2013043099A2 WO 2013043099 A2 WO2013043099 A2 WO 2013043099A2 SE 2012000139 W SE2012000139 W SE 2012000139W WO 2013043099 A2 WO2013043099 A2 WO 2013043099A2
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WO
WIPO (PCT)
Prior art keywords
particles
process according
average diameter
droplet
forming device
Prior art date
Application number
PCT/SE2012/000139
Other languages
English (en)
Other versions
WO2013043099A3 (fr
WO2013043099A8 (fr
Inventor
Ingemar Jonsson
Ralf Andersson
Lars Erik PAULSSON
Original Assignee
Ijorari Hb
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
Application filed by Ijorari Hb filed Critical Ijorari Hb
Publication of WO2013043099A2 publication Critical patent/WO2013043099A2/fr
Publication of WO2013043099A3 publication Critical patent/WO2013043099A3/fr
Publication of WO2013043099A8 publication Critical patent/WO2013043099A8/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes 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
    • B01J2/04—Processes 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/18—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using a vibrating apparatus
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0033—Shaping the mixture
    • C06B21/005—By a process involving melting at least part of the ingredients
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0033—Shaping the mixture
    • C06B21/0066—Shaping the mixture by granulation, e.g. flaking

Definitions

  • the particles are spherical and homogenous and mono disperse (i.e. of narrow particle size distribution, +/- 15 % of the mean particle diameter(s) main fraction(s)).
  • Optimum practical packaging density is obtained by packing a predetermined mix of two or more particle size fractions for good handling, function and performance.
  • fractions of spherical particles of the respective mean particle sizes/diameters 50 ⁇ and 200 ⁇ and of narrow particles size/diameter, distribution +/-15 % of the mean particle size(s) where e.g. 50 ⁇ particles fill the spaces between the larger particles, e.g. 200 ⁇ .
  • a general rule for optimal packing is achieved by the packing of particles with a narrow particle size distribution is that the smaller particle's diameter should be a factor 0, 1-0, 3 or more preferably 0, 2 of the mean size of the larger particle. Further 40-60% or more preferably 50% of the number of the respective particles should be of the respective mean particle size.
  • Today particles of e.g. Ammonium dinitramide (ADN) and other energetic materials are produced by prilling described e g in US 6610157, EP 0994 829 Bl and WO 9901408, where solid particulate ADN is introduced into the top of a melting column, allowed first to melt to form pre-prills while passing through a hot-zone ("heated zone") in the prilling column.
  • the pre-prills are allowed to become spherical in the presence of an upwardly blown inert medium which is counter current to the path of the ADN in the prilling column.
  • prills can be produced by emulsion, e g as described in EP 0953 55 Bl EP 1331213, EP 0953555 and WO 9747571.
  • a third alternative is spray prilling.
  • Spinning disk has been discussed for the production of Hydrazine Perchlorate prills, in US 3716315, where the disk is heated by overheating the melt. This is though not possible with ADN as ADN will decompose, including a risk of self-ignition, when overheated.
  • Decomposition is time/temperature dependent. To compensate for the cooling effect of the spinning disk, this has to be heated by e.g. electromagnetic induction heating under strict, preferably, feedback control as is done according to the present invention. Such continuous temperature control is not even suggested in '315.
  • control and similar terms is intended to encompass “monitor”, “adjust” and “correct” and similar terms.
  • particle size/diameter and particle size/diameter distribution fractions, shape and homogeneity have a vital importance for the practical handling, function and performance.
  • particle size/diameter and particle size/diameter distribution fractions, shape and homogeneity have a vital importance for the practical handling, function and performance.
  • a Spinning Disk drop generator is a rotating disc(s) over which the temperature is controlled.
  • a temperature controlled melt/liquid/slurry will under centrifugal force migrate towards the periphery where droplets are formed due to the specific melt's viscoelastic properties and density, which under precise control of the temperature of the rotation disc/discs, its angular rotation and mass flow.
  • mono disperse spherical particles i.e. spherical particles with narrow diameter distribution
  • Precise control of the disc temperature is achieved e g through electromagnetic induction heating and feedback control under e.g. an, contact free, ir-sensor.
  • Alternative heating of the disc can be performed via hot gas flow, such as a flow of air, preferably a flow of an inert gas, more preferably a flow of nitrogen, or IR-irradiation or combinations thereof.
  • melt is meant materials at temperatures above their solidification point alternatively solutions of materials that will solidify by evaporation of the solute or slurries of dispersed particles including binder(s) where the solute will evaporate after the droplet(s) were formed and spheres will stabilize by falling through air or an inert gas, preferably nitrogen.
  • the particles can be captured by falling into an organic solvent, e.g. Hexane, Dichloromethane, Butyl-acetate and low-volatile chloro-flouro-hydrocarbone (freons):
  • Trichlorofluoromethane l,l,2-Trichloro-l,2,2-trifluoroethane ⁇ l,l,l-Trichloro-2,2,2- trifluoroethane, 1,1-Dichloro-l-fluoroethane, 1,1,2-Trichlorotrifluoroethane, l-Bromo-2- chloro-l,l,2-trifluoroethane, l-Bromo-2-chloro-l,l,2-trifluoroethane, 2-Bromo-2-chloro- 1,1,1-trifluoroethane, l,l-Dichloro-2,2,3,3,3-pentafluoropropane, l,3-Dichloro-l,2,2,3,3- pentafluoropropane to stabilize.
  • Some of these solvents also offer excellent storage of energetic materials as they flameless and volatile at low temperatures, ⁇ 60°C.
  • An alternative surprising process for the droplet formation is via an Ultrasonic Atomizer, a concentrically mounted metal tube/channel extended at the outlet into a vertical horn(disc) designed into a tuning fork under pizoelectric oscillation controlled via a frequency modulator which under precise temperature, mass flow and frequency control is applied, resulting in generation of droplets of melts and slurries in much the same way as for the spinning disc, however with the difference that the throw distance resulting is considerably more narrow, less than 30cm as compared up to 3m for the spinning disk alternative. On the other hand is the possibility to control the respective particles fraction size(s) more limited.
  • Ultrasonic Atomizer Equipment available from Lechler Gmbh,Metzingen, Germany e.g. product types US1, US 10, US30, US50 in combination with an suitable Oscillator from the same company. Precise temperature control of the Ultrasonic Atomizer is achieved through electromagnetic induction heating and feedback control under one or several temperature sensors.
  • Alternative heating of the disc can be performed via hot gas flow, such as a flow of air, preferably a flow of an inert gas, more preferably a flow of nitrogen, or IR-irradiation or combinations thereof, preferably combinations being under feedback control under temperature sensor(s)
  • hot gas flow such as a flow of air, preferably a flow of an inert gas, more preferably a flow of nitrogen, or IR-irradiation or combinations thereof, preferably combinations being under feedback control under temperature sensor(s)
  • Spinning Disc/Ultra sound nozzle technologies offer the possibility to control and optimize the manufacturing of a melt resulting in spherical particles with narrow particle size distribution, +/-15 % of the mean particle size(s) and potentially very large production capacity over time.
  • Cellulose, ADN and Nitro Cellulose demonstrate that droplets and particles of limited particle distribution characterized with reliable reproducible results.
  • the production of spherical particles of narrow particle size/diameter distribution, +/-15 % of the mean particle size(s) Rotating Disc or Ultra Sound Nozzle result in excellent production capacity, utilization degree and reduce or eliminate the need for sieving.
  • the size/diameter is measured by light microscope.
  • Phase grade a Another parameter that effects the particle size distribution is Phase grade a. By adapting temperature, viscosity and the melts module of elasticity towards a high Phase grade a ( 70° - 90°) particle size distribution is controlled.
  • the peripheral distance is proportional to the production capacity and can be controlled via increased diameter of the disc alternatively a stacked multidisc, i.e. several discs mounted on top of each other on the same rotating axis.
  • the aforesaid is illustrated in below Diagram 1 and Table 1.
  • Example 1 A melt of Ammoniumdinitramide (ADN), alone or with addition of stabilizer or other energetic materials, was pumped at, at 28ml/min onto a spinning disc (Diam 20cm.
  • ADN Ammoniumdinitramide
  • ADN Ammoniumdinitramide
  • Urea particles were manufactured from an Urea melt as in Example 1, however at a temp of 134 2C and a continuously controlled temperature of 130 5 C, resulting in particles of a mean particle size of 50pm and a standard deviation of 7-10 ⁇ , with little or no need for sieving.
  • Example 10 Melted Urea at a temp of 130 9 C was kept in a thermo stated pan and was pumped through a thermo stated tube, lOOml/min, into an, by hot air, thermostated US1 Ultra sound Nozzle available from Lechler Gmbh,Metzingen, Germany, vibrating between 30-55 kHz. The atomized material was exposed to room temperature and led to fall 150cm into a bucket. Resulting in particles of mean particle sizes/diameters of 100 pm (vol 70%) and 25pm(vol 30%) with a standard deviation of 7-10pm, with little or no need for sieving.
  • Example 12 Nitrocellulose (NC) with added Stabiliser was dissolved in Methylethylketon (MEK) or in another NC-dissolving solvent to a viscous solution, 0.05-0.5 Pas, was pumped at, at
  • NC Nitrocellulose
  • MEK Methylethylketon
  • US1 Ultra sound Nozzle available from Lechler Gmbh,Metzingen, Germany, vibrating between 30-55 KHz.
  • the solvent MEK was removed from the droplets by help of an upward laminar air flow of 0,45 m/s +/- 20%, 20-40°C meeting the droplets on their way down falling to a reservoir of water.
  • NC Nitrocellulose
  • CAB Celluloseacetatebutyrate
  • MEK Methylethylketon
  • ⁇ finely ground Hexogen
  • the viscous solution 0.05-0.5 Pas, was fed to a spinning disc and droplets were formed when the liquid was leaving the rotation disc.
  • Spherical solid particles were formed after the droplets have been depleted of the solvent by help of an upward laminar air flow of 0,45 m/s +/- 20%, 20 - 40°C during their fall downwards to a reservoir of Water.
  • Example 15 Nitrocellulose (NC) and Celluloseacetatebutyrate (CAB) were dissolved in Methylethylketon (MEK) and finely ground Hexogen(RDX) ⁇ ⁇ , was added to the solution together with small amounts of Stabilizer. The viscous solution, 0.05-0.5 Pas, was pumped through an thermo stated tube, lOOml/min, into an, by hot air, thermo stated USl Ultra sound Nozzle available from Lechler Gmbh,Metzingen, Germany, vibrating between 30-55 kHz.
  • MEK Methylethylketon
  • RDX Hexogen
  • Spherical solid particles were formed after the droplets have been depleted of the solvent by help of an upward laminar air flow of 0,45 m/s +/- 20%, 20 - 40°C during their fall downwards to a reservoir of Water.
  • the received product of a blend of NC, CAB, Stabiliser and RDX, with a mean particle size of 50 ⁇ , with little or no need for sieving, is useful as a fast burning propellant after addition of Graphite for safe handling.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

La présente invention concerne un procédé pour fabriquer des particules à partir de matériau(x) énergétique(s) et/ou de matériau(x) de propulsion de telle manière que lesdites particules soient formées à partir de gouttelettes dudit/desdits matériau(x) sous forme de matière fondue. La température d'un dispositif de formation de gouttelettes ainsi utilisé est régulée en continu. Lesdites gouttelettes sont solidifiées en lesdites particules pendant la chute.
PCT/SE2012/000139 2011-09-22 2012-09-17 Procédé pour fabriquer des particules et particules fabriquées ainsi WO2013043099A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE1100693-9 2011-09-22
SE1100693 2011-09-22

Publications (3)

Publication Number Publication Date
WO2013043099A2 true WO2013043099A2 (fr) 2013-03-28
WO2013043099A3 WO2013043099A3 (fr) 2013-06-20
WO2013043099A8 WO2013043099A8 (fr) 2013-11-07

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112657420A (zh) * 2020-11-24 2021-04-16 江苏方圆芳纶研究院有限公司 一种球形苯二甲酰氯颗粒及其制造方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3716315A (en) * 1965-10-19 1973-02-13 Aerojet General Co Novel apparatus for the production of anhydrous spherical ammonium perchlorate useful in rocket propellants
WO1999021795A1 (fr) * 1997-10-28 1999-05-06 Försvarets Forskningsanstalt Procede de production de granules de dinitramide d'ammonium (adn)
EP0994829B1 (fr) * 1997-07-02 2004-03-17 Alliant Techsystems Inc. Particules de dinitramide d'ammonium perlees thermiquement stabilisees et procede de stabilisation de ces dernieres
DE102007003396A1 (de) * 2006-02-14 2007-08-30 Deutsch Französisches Forschungsinstitut Saint Louis Nanokristallisations-Verfahren

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3716315A (en) * 1965-10-19 1973-02-13 Aerojet General Co Novel apparatus for the production of anhydrous spherical ammonium perchlorate useful in rocket propellants
EP0994829B1 (fr) * 1997-07-02 2004-03-17 Alliant Techsystems Inc. Particules de dinitramide d'ammonium perlees thermiquement stabilisees et procede de stabilisation de ces dernieres
WO1999021795A1 (fr) * 1997-10-28 1999-05-06 Försvarets Forskningsanstalt Procede de production de granules de dinitramide d'ammonium (adn)
DE102007003396A1 (de) * 2006-02-14 2007-08-30 Deutsch Französisches Forschungsinstitut Saint Louis Nanokristallisations-Verfahren

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112657420A (zh) * 2020-11-24 2021-04-16 江苏方圆芳纶研究院有限公司 一种球形苯二甲酰氯颗粒及其制造方法

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WO2013043099A3 (fr) 2013-06-20
WO2013043099A8 (fr) 2013-11-07

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