EP0052552A1 - Verfahren zur Herstellung feiner Treibpulver durch Granulation und so hergestellte Pulver - Google Patents

Verfahren zur Herstellung feiner Treibpulver durch Granulation und so hergestellte Pulver Download PDF

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Publication number
EP0052552A1
EP0052552A1 EP81401750A EP81401750A EP0052552A1 EP 0052552 A1 EP0052552 A1 EP 0052552A1 EP 81401750 A EP81401750 A EP 81401750A EP 81401750 A EP81401750 A EP 81401750A EP 0052552 A1 EP0052552 A1 EP 0052552A1
Authority
EP
European Patent Office
Prior art keywords
solvent
powders
granules
rounder
granulation
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
EP81401750A
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English (en)
French (fr)
Other versions
EP0052552B1 (de
Inventor
Yves Bertrand
Rémy Favrot
Pierre Gaudilliere
Jean-Charles Perennou
Bernard Wiedemann
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.)
Societe Nationale des Poudres et Explosifs
Original Assignee
Societe Nationale des Poudres et Explosifs
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.)
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Publication date
Application filed by Societe Nationale des Poudres et Explosifs filed Critical Societe Nationale des Poudres et Explosifs
Priority to AT81401750T priority Critical patent/ATE7221T1/de
Publication of EP0052552A1 publication Critical patent/EP0052552A1/de
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Publication of EP0052552B1 publication Critical patent/EP0052552B1/de
Expired legal-status Critical Current

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Classifications

    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S149/00—Explosive and thermic compositions or charges
    • Y10S149/118—Gel contains resin

Definitions

  • the present invention relates to the field of propellant powders in grains. More precisely, the present invention relates on the one hand to a new process for the production of fine granular powders by granulation of the basic energetic materials in a granulating tray, and on the other hand as new industrial products the fine propellant powders obtained thanks to this new process.
  • Fine propellants for small arms are, as a general rule, nitrocellulose-based powders produced according to the so-called solvent process.
  • nitrocellulose possibly mixed with other energy bases, is kneaded with solvents until it forms a homogeneous paste which is then spun with the press and cut into grains which are then wrung out, soaked, dried, smoothed and graphics if applicable.
  • This process is well described in the work of MM. Louis VENNIN, E. BURLOT and H. LECORCHE, "Les Poudres et Explosifs", published in 1932 at the Librairie Polytechnique Ch. BERANGER, pages 578 et seq.
  • porous powders are brighter than non-porous powders and that for many applications porous powders are sought despite the additional disadvantage of their manufacture.
  • the liveliness of a powder characterizes both its speed of combustion and the quantity of gas emitted in a given time of combustion.
  • This method has the advantage of allowing large production rates, but has the major drawback of consuming a lot of energy because it requires heating large amounts of water, moreover it has drawbacks in terms of pollution due to the large quantities of gum-containing water that is left as a by-product.
  • the object of the present invention is precisely to provide a simple and inexpensive method of manufacturing fine propellant powders in grains for small arms and which have good vivacity.
  • the method according to the invention consists in carrying out in a rotating apparatus the granulation of the base materials, sprayed with solvent, in carrying out a first partial drying of the granules thus obtained and in finishing the finishing of said granules in a rounder in the possible presence of solvent.
  • the method according to the invention can be carried out batchwise or continuously depending on the needs and capacities of the available equipment.
  • the invention also relates, as a new industrial product, to the propellant powders in grains obtained using the process according to the invention.
  • FIG. 1 schematically represents the installation necessary for the continuous implementation of the method according to the invention.
  • FIG. 2 is a diagram indicating all the operations necessary in an example of continuous manufacturing according to the invention.
  • the process according to the invention firstly consists in carrying out in a rotating apparatus the granulation of the finely ground base materials sprayed with a solvent.
  • the finely ground base materials are thus agglomerated using solvent in the form of granules of essentially spherical shape.
  • the rotating device is advantageously a "granulator tray” also sometimes called “pellet plate” widely used in the fertilizer or cement industry, but any equivalent device can also be used.
  • the granulator tray is regularly supplied with base material and the solvent is sprayed very finely onto the granules being formed.
  • the basic recovery materials are ground very finely, the average diameter of the ground particles being preferably less than 300 microns for weapons of common calibers.
  • the grinding takes place under water as well as the mixing of the ground materials and the unground materials.
  • the mixture of base materials is then drained to a degree of humidity of between 10 and 30% and preferably close to 20% before passing over the granulator tray.
  • the agglomeration of the basic materials on the granulator tray is done using a solvent. All the solvents of one of the solid bases can be used, but preference is given, for reasons of convenience of recovery, to the solvents which are insoluble or poorly soluble in water. This is how we will use as solvents when we are in the presence of nitrocellulose, ketones such as methyl ethyl ketone, methyl isobutyl ketone, esters such as ethyl acetate, acetate d isopropyl, isobutyl acetate, nitroparaffins such as nitromethane.
  • ketones such as methyl ethyl ketone, methyl isobutyl ketone
  • esters such as ethyl acetate, acetate d isopropyl, isobutyl acetate
  • nitroparaffins such as nitromethane.
  • a diluent is added to the solvent which must be non-solvent for nitrocellulose, but soluble in the solvent used.
  • diluent of light hydrocarbons such as white spirit or petrol A which is a petrol containing less than 1% of aromatic compounds and at least 80% of linear aliphatic hydrocarbons and the distillation temperature of which is between 40 and 100 ° C.
  • white spirit or petrol A which is a petrol containing less than 1% of aromatic compounds and at least 80% of linear aliphatic hydrocarbons and the distillation temperature of which is between 40 and 100 ° C.
  • the granules Upon leaving the granulator tray, the granules then undergo a first partial drying intended to remove part of the water. and solvents and are then terminated in a rounder in the possible presence of solvent.
  • the first drying can be carried out either in a conventional dryer, or in equivalent installations such as for example a fluidized bed.
  • the granules are then finished in a rounder, this latter operation being absolutely necessary for obtaining a propellant powder in grains having acceptable properties.
  • Rounder means any rotating device, whether or not provided with stirring tools, in which the outer surface of the granules is worked. It is advantageous to use as a rounder a granulating plate similar to that used for the actual granulation, but it is also possible to use any other commercial device fulfilling the desired function. In the case of a discontinuous process, it is advantageously possible to use as a rounder the granulator plate used for the granulation of the basic materials.
  • the rounding treatment is advantageously carried out in the presence of solvent and possibly of diluent.
  • Advantage can be taken of the passage through the rounder to add the constituents which can be fixed to the surface of the grains such as for example combustion moderators or anti-static agents such as graphite.
  • the total watering rate in solvent, excluding diluent, between the granulator plate and the rounder is generally between 60 and 140% by weight relative to the weight of dry base material to be treated and is preferably between 80 and 120 %.
  • the solvent / diluent weight ratio is preferably between 90/10 and 70/30.
  • the granules leaving the rounder are wrung and dried.
  • Spinning consists essentially of removing the solvent and optionally the diluent and is preferably carried out at room temperature while drying essentially consists of removing the water contained in the granules and is preferably carried out with hot air.
  • the granules are then sieved, the granules having the desired particle size are stored while the others are recycled after possibly undergoing grinding under water.
  • a first sieving can advantageously take place after the first drying and before the treatment in the rounder.
  • FIG. 1 schematically represents an installation necessary for the continuous implementation of the method according to the invention.
  • a storage tank 21 contains the basic materials which must be ground in the crusher 23. After grinding, these materials are mixed in the hopper 24 with the materials which do not require prior grinding from the storage tank 22.
  • the mixture basic material is transported by means of a conveyor belt 25 onto a heavy belt 26 and from there into a crumbler 27 before falling into a granulator plate 11 sprayed with a solvent coming from the tank 35.
  • the granules formed are recovered on a conveyor belt 12 and pass over a sieve 13 before undergoing a first drying in a fluidized bed 14, they are then conveyed by a conveyor belt 15 in a rounder 16, at their exit from the rounder 16 the granules are transported by a conveyor belt 17 in a storage hopper 18 before undergoing the last treatments.
  • FIG. 2 is a diagram representing a possibility of complete implementation of the continuous process according to the invention.
  • the basic materials are stored in storage tanks 21 and 22.
  • the basic materials stored in the tank 21 are ground under water in the crusher 23 before being mixed in the mixer 24 with the materials coming from the tank 22.
  • the mixture of materials of base then undergoes partial elimination of the water in the dryer 26 so as to have a suitable humidity and then passes through the emitter 27 before being introduced into the granulator tray 11.
  • the tray 11 is sprayed with a liquid coming from a mixing tank 35 supplied from four tanks 31, 32, 33 and 34 respectively containing the plasticizer in solution, the solvent, the diluent and the stabilizer in solution.
  • a liquid coming from a mixing tank 35 supplied from four tanks 31, 32, 33 and 34 respectively containing the plasticizer in solution, the solvent, the diluent and the stabilizer in solution.
  • the granules are sieved on the sieve 13 and undergo a first drying in the fluidized bed 14 before being reprocessed in the rounder 16.
  • the rounder 16 is supplied with liquid from a tank mixture 36 containing solvent and diluent from tanks 32 and 33 as well as the combustion moderator from tank 37.
  • Graphite from a tank 38 is also added continuously to the rounder.
  • the granules are drained and then dried in the enclosure 41 before being screened on the screen 42.
  • the solvents are recovered and recycled to the mixing tank 35.
  • the granules having a correct particle size are stored in a hopper 43 while the finest granules are recycled into the mixer 24 and the largest granules are sent to the mill 23.
  • the invention also relates, as a new industrial product, to the fine propellant powders obtained by the process according to the invention. It is indeed one of the surprising aspects of the invention to allow the production of propellant powder grains of good liveliness without the use of soluble salt.
  • the grains of powders are obtained at the exit of the rounder and it is also surprising to note that the first passage on the granulator plate does not allow obtaining a propellant powder correctly adjusted but that it is only after a first drying and treatment in the rounder that a product is obtained having the characteristics of a propellant powder usable in small and medium caliber commercial weapons and mainly in hunting rifles.
  • the powders according to the invention can be described as heterogeneous in the sense that when viewed in section under a microscope, a homogeneous mass is not observed but a slightly porous heterogeneous mass is observed in which the elements belonging to each of the materials are recognized individually. basic.
  • the base material has a humidity of 20%, and the solvent used is ethyl acetate with a watering rate of 98%.
  • These basic materials are granulated in a granulating tray having a diameter of 600 mm and a plate height of 200 mm.
  • the plane of rotation of the plate is inclined by 62 ° relative to the plane of the horizontal and the speed of rotation of the plate is 24 revolutions / minute.
  • the feed rate of the granulator tray is 6 kg / hour of dry counted base material.
  • the granules obtained are dried for 3 hours at room temperature and are then reprocessed in a second granulator tray similar to the first and under the same conditions of flow rate and speed of rotation.
  • the humidity is 20% and the solvent used is butyl acetate.
  • This cake is granulated in a granulating tray having a diameter of 1,200 mm and a height of plate of 250 mm.
  • the plane of rotation of the plate is inclined by 57 ° relative to the plane of the horizontal and the speed of rotation is 20 revolutions per minute.
  • the feed rate is 12 kg / hour of dry counted base material with a watering rate of 72%.
  • the granules are dried for 3 hours at room temperature and are then reprocessed in a second granulator tray under similar conditions.
  • This example shows the influence of too high a moisture content in the base materials on the performance of the powder.
  • the humidity level of the cake is 40%, the solvent used is methyl ethyl ketone with a watering rate of 140%.
  • a powder is thus obtained having a potential of 1045 cal / g but whose grain vivacity for the particle size cutting between 800 and 1600 microns is too high for normal use in a hunting weapon. This powder could be suitable for very specific applications, for example for very low lead charges.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Glanulating (AREA)
  • Medicinal Preparation (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
EP81401750A 1980-11-14 1981-10-30 Verfahren zur Herstellung feiner Treibpulver durch Granulation und so hergestellte Pulver Expired EP0052552B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81401750T ATE7221T1 (de) 1980-11-14 1981-10-30 Verfahren zur herstellung feiner treibpulver durch granulation und so hergestellte pulver.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8024187A FR2494263A1 (fr) 1980-11-14 1980-11-14 Procede de fabrication de poudres propulsives fines par granulation et poudres ainsi obtenues
FR8024187 1980-11-14

Publications (2)

Publication Number Publication Date
EP0052552A1 true EP0052552A1 (de) 1982-05-26
EP0052552B1 EP0052552B1 (de) 1984-04-25

Family

ID=9247959

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81401750A Expired EP0052552B1 (de) 1980-11-14 1981-10-30 Verfahren zur Herstellung feiner Treibpulver durch Granulation und so hergestellte Pulver

Country Status (17)

Country Link
US (1) US4444606A (de)
EP (1) EP0052552B1 (de)
AR (1) AR243147A1 (de)
AT (1) ATE7221T1 (de)
AU (1) AU543481B2 (de)
BR (1) BR8107382A (de)
CA (1) CA1187292A (de)
DE (1) DE3163321D1 (de)
ES (1) ES507058A0 (de)
FI (1) FI73660C (de)
FR (1) FR2494263A1 (de)
GR (1) GR76326B (de)
MA (1) MA19329A1 (de)
MT (1) MTP903B (de)
NZ (1) NZ198924A (de)
OA (1) OA06948A (de)
YU (1) YU41996B (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2233972A (en) * 1989-04-18 1991-01-23 Royal Ordnance Plc Propellant powders
EP0458439A2 (de) * 1990-05-24 1991-11-27 Trw Vehicle Safety Systems Inc. Verfahren zum Kugeligglühen

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3242301A1 (de) * 1982-11-16 1984-05-17 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V., 8000 München Verfahren und vorrichtung zur herstellung ein- oder mehrbasiger treibladungspulver
BR8405016A (pt) * 1984-10-04 1986-05-13 Charles Helle Processo para a preparacao de polvoras propelentes
US4764329A (en) * 1987-06-12 1988-08-16 The United States Of American As Represented By The Secretary Of The Army Producing explosive material in granular form
US5156779A (en) * 1989-04-27 1992-10-20 E. I. Du Pont De Nemours And Company Process and apparatus for producing ultrafine explosive particles
US5198616A (en) * 1990-09-28 1993-03-30 Bei Electronics, Inc. Frangible armor piercing incendiary projectile
US5472647A (en) * 1993-08-02 1995-12-05 Thiokol Corporation Method for preparing anhydrous tetrazole gas generant compositions
AU7553794A (en) * 1993-08-02 1995-02-28 Thiokol Corporation Method for preparing anhydrous tetrazole gas generant compositions
US9409825B2 (en) 2013-08-20 2016-08-09 Los Alamos National Security, Llc Granulation of fine powder
RU2602904C2 (ru) * 2015-04-16 2016-11-20 Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") Способ получения двухосновного сферического пороха для стрелкового оружия
FR3064639B1 (fr) 2017-03-30 2020-07-24 Eurenco France Films d'ethylcellulose et blocs de propergol double-base inhibes en combustion avec de tels films

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE117349C (de) *
US1752881A (en) * 1924-03-01 1930-04-01 American Powder Company Manufacture of smokeless powder

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3329743A (en) * 1963-05-15 1967-07-04 Olin Mathieson Lacquer process for preparing small diameter nitrocellulose particles
US3236702A (en) * 1964-04-08 1966-02-22 Hercules Powder Co Ltd Manufacture of densified spheroidal fine particle nitrocellulose
US3325571A (en) * 1966-01-25 1967-06-13 Hercules Inc Process for the manufacture of smokeless powder
US3563977A (en) * 1968-02-28 1971-02-16 Du Pont Granular nitrocellulose manufacture
US3671342A (en) * 1970-01-02 1972-06-20 Atlas Chem Ind Dynamite composition containing expanded thermoplastic beads
US3711343A (en) * 1971-08-20 1973-01-16 Us Army Cellular nitrocellulose based composition and method of making

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE117349C (de) *
US1752881A (en) * 1924-03-01 1930-04-01 American Powder Company Manufacture of smokeless powder

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
TENNEY L. DAVIS: " The Chemistry of Powder and Explosives ", 1943 John Wiley & Sons, pages 287-292 New York, US * page 287, alinea 2; page 288 dernier alinea - page 289, ligne 7; page 289, ligne 22 - page 290, ligne 34 * *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2233972A (en) * 1989-04-18 1991-01-23 Royal Ordnance Plc Propellant powders
EP0458439A2 (de) * 1990-05-24 1991-11-27 Trw Vehicle Safety Systems Inc. Verfahren zum Kugeligglühen
EP0458439A3 (en) * 1990-05-24 1992-10-21 Trw Vehicle Safety Systems Inc. Spheronizing process

Also Published As

Publication number Publication date
FI73660C (fi) 1987-11-09
EP0052552B1 (de) 1984-04-25
GR76326B (de) 1984-08-04
ES8304050A1 (es) 1983-03-01
FI813591L (fi) 1982-05-15
MTP903B (en) 1985-01-17
ES507058A0 (es) 1983-03-01
CA1187292A (en) 1985-05-21
BR8107382A (pt) 1982-08-10
NZ198924A (en) 1985-04-30
DE3163321D1 (en) 1984-05-30
AR243147A1 (es) 1993-07-30
FR2494263A1 (fr) 1982-05-21
FI73660B (fi) 1987-07-31
AU7738981A (en) 1982-05-20
AU543481B2 (en) 1985-04-18
OA06948A (fr) 1983-07-31
US4444606A (en) 1984-04-24
FR2494263B1 (de) 1983-08-19
YU268481A (en) 1983-10-31
YU41996B (en) 1988-04-30
MA19329A1 (fr) 1982-07-01
ATE7221T1 (de) 1984-05-15

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