EP0001526A1 - Verfahren zur Entfernung in einem flüssigen Wasser-Alkohol Medium von in Treibpulverkörnern enthaltenen Lösungsmitteln - Google Patents

Verfahren zur Entfernung in einem flüssigen Wasser-Alkohol Medium von in Treibpulverkörnern enthaltenen Lösungsmitteln Download PDF

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Publication number
EP0001526A1
EP0001526A1 EP78400114A EP78400114A EP0001526A1 EP 0001526 A1 EP0001526 A1 EP 0001526A1 EP 78400114 A EP78400114 A EP 78400114A EP 78400114 A EP78400114 A EP 78400114A EP 0001526 A1 EP0001526 A1 EP 0001526A1
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EP
European Patent Office
Prior art keywords
powder
hydroalcoholic
liquid phase
phase
grains
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
EP78400114A
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English (en)
French (fr)
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EP0001526B1 (de
Inventor
Louis Leneveu
Paul Seite
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
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Publication date
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Publication of EP0001526A1 publication Critical patent/EP0001526A1/de
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Publication of EP0001526B1 publication Critical patent/EP0001526B1/de
Expired legal-status Critical Current

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    • 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
    • C06B21/0091—Elimination of undesirable or temporary components of an intermediate or finished product, e.g. making porous or low density products, purifying, stabilising, drying; Deactivating; Reclaiming

Definitions

  • the present invention relates to a method for removing the solvents contained in the propellant powders in grains manufactured according to the so-called "solvent" method, when said solvents consist of an ether-alcohol mixture.
  • grain powders are understood to mean both powders in the form of cylindrical grains and those in the form of strips or flakes.
  • the propellant powders in grains manufactured according to the so-called "solvent" process are generally either powders with a simple nitrocellulose base, or powders of which at least a part of the energetic material consists of nitrocellulose, the remainder of the energetic material consisting of solid organic propellant bases well known to those skilled in the art, such as, for example, polyvinyl nitrate, cellulose acetate, polyvinyl acetate, etc. or mixtures of these bodies.
  • the conventional spinning operation at room temperature or slightly above room temperature has a major drawback: the partial pressures of ether and alcohol being close to this temperature range, the two solvents evaporate at the same time time.
  • the molecules contained on the surface of a grain evaporate more easily than those contained in the heart of the grain.
  • the evaporation of the ether can cause condensation of the water on the surface of the grain, which leads to a reprecipitation of the nitrocellulose on the surface, so a film forms on the surface of the powder grain. makes the diffusion of the solvents contained in the core of the powder grain more difficult. It is this phenomenon which explains the necessity of the long duration of the so-called soaking operation, the durations of which, in hot water, are in many cases close to 150 hours.
  • the object of the present invention is to remedy the aforementioned drawbacks by proposing a new process for eliminating the solvents contained in the grains of propellant powders produced according to a process with solvents in which said solvents are constituted by the mixture of an ether and of '' an alcohol, a process which ensures the elimination of ether so as to avoid any film formation on the surface of the powder grains and to allow a reduction of the soaking time and consequently an increase in the chemical stability of the powder by less degradation of the latter.
  • this result is achieved by performing a selective elimination of the ether contained in the powder grains by immersion of the latter in a hydroalcoholic liquid medium in which a gas is bubbled.
  • the process for removing solvents according to the invention thus has the direct consequence of reducing the duration of the subsequent soaking and, as an indirect consequence, a gain in the chemical stability of the powder grain, as well as better reproducibility of the powder thanks to the the fact that the solvent removal conditions can be repeated almost identically.
  • the method according to the invention also allows a reduction in the intermediate handling that a conventional soaking required.
  • the ether contained in the powder grains produced according to the so-called solvent process is removed, the said solvents being constituted by the mixture of an alkanol and an ether of alkyl, by immersion of said grains of powders in a hydroalcoholic liquid phase in which a gas circulates, said hydroalcoholic phase being constituted by an aqueous dilution of the alkanol used as solvent for said powder, in proportions such that said title hydroalcoholic liquid phase between 20 and 70 degrees Gay-Lussac, the temperature of said hydroalcoholic phase being between 10 and 40 ° C.
  • Said gas can simply be air or an inert gas which is a good carrier of said ether, such as nitrogen. It may be advantageous, in the case of large installations in order to eliminate any risk of detonation, to start the elimination of the ether using such an inert gas and to finish said elimination either with said inert gas, more simply with air.
  • the ratio of the mass of powder to be treated to the mass of the hydroalcoholic liquid phase to be used must be less than or equal to one and preferably close to 1/3.
  • the hydroalcoholic liquid phase must titrate between 20 and 70 degrees Gay-Lussac and preferably between 30 and 50 degrees Gay-Lussac, its temperature must be between 10 and 40 ° C and preferably between 15 and 25 ° C.
  • any apparatus can be used to ensure the circulation of a gas in a liquid phase such as for example a reactor provided with one or more inlets for the gas which must circulate in the liquid phase.
  • the apparatus is equipped with an agitator such as for example an anchor or propeller agitator.
  • said apparatus is surrounded by a thermostatically controlled enclosure so as to be able to properly control the temperature in the implementation of the method according to the invention.
  • the grains of powders can either be subjected to short-term soaking and be smoothed and / or graphitized according to conventional techniques or else be subjected to smoothing-soaking in an aqueous liquid medium as described in the French patent application. n ° 77.11938 in the name of the plaintiff with possibly a later graphitization.
  • powder B 19 T is a simple nitrocellulose base powder, in the form of small cylinders 3 mm in diameter and 4 mm long axially drilled with 19 holes.
  • the composition of this powder on kneading is as follows: After cutting the powder grains still contain 21% by weight of ethyl ether and 15% by weight of ethyl alcohol. The grains were divided into two lots:
  • This apparatus consists of a thermostatically controlled enclosure 1 constituting, by its shape, a reactor, said enclosure being supplied by a regulating fluid 2.
  • a pipe 3 allows the arrival of the bubbling gas 4.
  • the powder and the liquid phase are agitated by means of the agitator 7.
  • the interior volume of the reactor is 35 liters and its internal diameter 30 cm.
  • the powder grains contained 10% by weight of ethyl alcohol and 0.10% by weight of ethyl ether, the percentages being expressed relative to the total weight of the dry matter.
  • the powder grains of batch B were spun in a conventional manner at normal pressure at the rate of 8 hours in a rack at room temperature and 20 hours in a box at 30 ° C with an additional hour of cooling.
  • the powders of the two batches were smoothed with centralite (symmetrical diethyl diphenyl urea) and graphitized according to the usual techniques known to those skilled in the art.
  • the powders of the two batches were fired into a 30 mm gun, the shell weighed 235 grams and the powder charge was 48.2 grams.
  • a powder treated according to the invention gives firing results entirely comparable to those provided by the same powder treated in a conventional manner but that the first has a chemical stability greater than the second at low temperature, which shows that nitrocellulose has been less degraded in a powder treated according to the invention than in a powder treated in a conventional manner.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Extraction Or Liquid Replacement (AREA)
EP78400114A 1977-10-03 1978-09-26 Verfahren zur Entfernung in einem flüssigen Wasser-Alkohol Medium von in Treibpulverkörnern enthaltenen Lösungsmitteln Expired EP0001526B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR7729683 1977-10-03
FR7729683A FR2404612A1 (fr) 1977-10-03 1977-10-03 Procede d'elimination en milieu liquide hydroalcoolique des solvants contenus dans les poudres propulsives en grains

Publications (2)

Publication Number Publication Date
EP0001526A1 true EP0001526A1 (de) 1979-04-18
EP0001526B1 EP0001526B1 (de) 1981-04-29

Family

ID=9196037

Family Applications (1)

Application Number Title Priority Date Filing Date
EP78400114A Expired EP0001526B1 (de) 1977-10-03 1978-09-26 Verfahren zur Entfernung in einem flüssigen Wasser-Alkohol Medium von in Treibpulverkörnern enthaltenen Lösungsmitteln

Country Status (4)

Country Link
EP (1) EP0001526B1 (de)
DE (1) DE2860662D1 (de)
FR (1) FR2404612A1 (de)
IT (1) IT7869272A0 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0622605A1 (de) * 1993-04-27 1994-11-02 Neyrpic Framatome Mecanique Verfahren und automatische Einrichtung zur Delaborierung von chemischer Munitionen
FR2704640A1 (fr) * 1993-04-26 1994-11-04 Snpe Ingenierie Sa Procédé et installation de destruction de munitions contenant des agents toxiques.

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2691800A (en) * 1951-02-10 1954-10-19 Olin Ind Inc Method of recovering explosives in particular form
FR1185754A (fr) * 1957-11-05 1959-08-05 Le Secretaire D Etat A La Defe Procédé d'élimination et de récupération des dissolvants utilisés dans la fabrication des poudres ou d'autres produits industriels
US3622655A (en) * 1969-04-14 1971-11-23 Hercules Inc Aqueous slurry process for drying of solvent wet double base smokeless powder
FR2244731A1 (de) * 1973-09-20 1975-04-18 Bofors Ab

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2691800A (en) * 1951-02-10 1954-10-19 Olin Ind Inc Method of recovering explosives in particular form
FR1185754A (fr) * 1957-11-05 1959-08-05 Le Secretaire D Etat A La Defe Procédé d'élimination et de récupération des dissolvants utilisés dans la fabrication des poudres ou d'autres produits industriels
US3622655A (en) * 1969-04-14 1971-11-23 Hercules Inc Aqueous slurry process for drying of solvent wet double base smokeless powder
FR2244731A1 (de) * 1973-09-20 1975-04-18 Bofors Ab

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2704640A1 (fr) * 1993-04-26 1994-11-04 Snpe Ingenierie Sa Procédé et installation de destruction de munitions contenant des agents toxiques.
US5574203A (en) * 1993-04-26 1996-11-12 Snpe Ingenierie S.A. Process and installation for destroying munitions containing toxic agents
EP0622605A1 (de) * 1993-04-27 1994-11-02 Neyrpic Framatome Mecanique Verfahren und automatische Einrichtung zur Delaborierung von chemischer Munitionen
FR2704641A1 (fr) * 1993-04-27 1994-11-04 Neyrpic Framatome Mecanique Procédé et installation automatique de neutralisation de munitions chimiques.

Also Published As

Publication number Publication date
FR2404612A1 (fr) 1979-04-27
DE2860662D1 (en) 1981-08-06
FR2404612B1 (de) 1980-02-08
EP0001526B1 (de) 1981-04-29
IT7869272A0 (it) 1978-10-02

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