EP1427683A2 - Compositions pyrotechniques solides absorbant peu l'humidite et procedes de production de ces dernieres - Google Patents

Compositions pyrotechniques solides absorbant peu l'humidite et procedes de production de ces dernieres

Info

Publication number
EP1427683A2
EP1427683A2 EP02789146A EP02789146A EP1427683A2 EP 1427683 A2 EP1427683 A2 EP 1427683A2 EP 02789146 A EP02789146 A EP 02789146A EP 02789146 A EP02789146 A EP 02789146A EP 1427683 A2 EP1427683 A2 EP 1427683A2
Authority
EP
European Patent Office
Prior art keywords
pyrotechnic composition
solid pyrotechnic
weight percent
composition according
particles
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.)
Withdrawn
Application number
EP02789146A
Other languages
German (de)
English (en)
Inventor
Reed J. Blau
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.)
Northrop Grumman Innovation Systems LLC
Original Assignee
Alliant Techsystems Inc
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 Alliant Techsystems Inc filed Critical Alliant Techsystems Inc
Publication of EP1427683A2 publication Critical patent/EP1427683A2/fr
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
    • C06C9/00—Chemical contact igniters; Chemical lighters
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
    • C06B31/02—Compositions containing an inorganic nitrogen-oxygen salt the salt being an alkali metal or an alkaline earth metal nitrate
    • C06B31/08—Compositions containing an inorganic nitrogen-oxygen salt the salt being an alkali metal or an alkaline earth metal nitrate with a metal oxygen-halogen salt, e.g. inorganic chlorate, inorganic perchlorate
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
    • C06B31/28—Compositions containing an inorganic nitrogen-oxygen salt the salt being ammonium nitrate
    • C06B31/30—Compositions containing an inorganic nitrogen-oxygen salt the salt being ammonium nitrate with vegetable matter; with resin; with rubber

Definitions

  • the present invention is directed to solid pyrotechnic compositions, including novel black powder substitute and boron/potassium nitrate substitute compositions.
  • the present invention is also directed to methods for making the solid pyrotechnic compositions.
  • Black powder and boron/potassium nitrate are two classic igniter formulations with broad current usage in a wide variety of applications.
  • Black powder is composed of 72-75 weight percent potassium nitrate, 15-18 weight percent charcoal, and 10 weight percent sulfur. Variations in this basic black powder formulation are known.
  • the optimum formulation for black powder is generally accepted to consist of 75 weight percent potassium nitrate, 15 weight percent charcoal, and 10 weight percent sulfur. Black powder of this formulation has a predicted flame temperature of 1950K at 1000 psi.
  • Boron/potassium nitrate on the other hand, in its optimum formulation is composed of 75 weight percent potassium nitrate and 25 weight percent boron.
  • boron/potassium nitrate has a significantly higher flame temperature of 3034K at 1000 psi.
  • B/KNO3 common applications for B/KNO3 include ignition trains for rockets, decoy flares, and gas generators of automotive secondary safety restraints or "air bag” devices.
  • Boron/potassium nitrate is not, however, used as often in multi-use hardware due to the expense of BKNO3 and the high BKNO3 flame temperature, which may cause premature erosion of reusable hardware.
  • charcoal and sulfur may be ball milled together into an intimate mixture for feeding into an extruder. Ball milling also serves to reduce the particle size of the charcoal. Potassium nitrate is dried and likewise processed through a rod mill to reduce the average particle size to about 50 microns.
  • Graphite may optionally be introduced into the rod mill for the purpose of reducing electrostatic discharge sensitivity (ESD). The milled charcoal, sulfur, and potassium nitrate, and optionally the graphite, are then compounded in accordance with well known methods.
  • Sulfur dioxide is extremely destructive to tissue of the mucous membranes and upper respiratory tract, eyes, and skin. Inhalation may result in spasm, inflammation, and edema of the larynx and bronchi, chemical pneumonitis, and pulmonary edema. Thus, exposure to sulfur dioxide can lead to a series of health problems and, in the case of extended exposure, death.
  • the charcoal constituent of black powder imparts a degree of unpredictability to the performance of the igniter composition.
  • Charcoal is produced by carbonization of wood.
  • the chemical and physical properties of wood vary greatly, depending upon the particular properties of the tree species, soil composition, and environmental conditions from which the wood is taken. Due to inherent variability of wood and fluctuations in the carbonization process, the properties of charcoal tend to vary from batch to batch. These variations can affect the consistency of black powder performance.
  • Black powder absorbs about 1.5 weight percent moisture under 75 percent relative humidity at 21.1°C (70°F) over the period of 24 hours. If black powder picks up sufficient moisture, there is a possibility that the black powder will not burn as fast. Hence, an igniter or other device comprising the black powder might not perform up to specification in a high relative humidity. Also, concerns have been expressed that water will cause the potassium nitrate to migrate out of the black powder pellet and cause corrosion of metallic parts of the device.
  • a black powder substitute composition is described in U.S. Patent No. 5,320,691 to Weber.
  • This composition is a dispersion of phenolphthalein, potassium nitrate, and sulfur in a binding phase of phenolphthalein salt.
  • Phenolphthalein is the reaction product of a phenolic compound and phthalic anhydride.
  • the cations of the phenolphthalein salt are selected from the group consisting of sodium, potassium, lithium, and ammonium.
  • Phenolphthalein salt (optionally in combination with organic phenolphthalein) is used because of the ballistic enhancement that the phenolphthalein salt imparts in comparison to organic phenolphthalein.
  • the solid pyrotechnic composition contains 75 weight percent potassium nitrate, 10 weight percent elemental sulfur, and 15 weight percent crystalline compound.
  • the crystalline compound may be fluorescein, phenolphthalein, 1,5-naphthalenediol, anthraflavic acid, terephthalic acid, and alkali metal salts thereof.
  • H72 relies on elemental sulfur for minimizing the ignition delay of the igniter.
  • an organic crystalline compound includes in its definition not only a single organic crystalline compound, but also a combination of two or more organic crystalline compounds.
  • polymer encompasses homopolymers, copolymers, and terpolymers.
  • Terpolymer means a polymer made from three or more monomers.
  • organic crystalline compound means an organic compound that is not present as a salt, unless the term in the context clearly dictates otherwise.
  • a salt of an organic crystalline compound means a negatively charged organic compound ionically bonded to a metal cation or ammonium cation to counterbalance the negative charge of the organic compound.
  • An example is dipotassium phenolphthalein.
  • a solid pyrotechnic composition constituting a black powder substitute for attaining the above and other objects.
  • the composition comprises about 40 weight percent to about 90 weight percent oxidizer particles having a mean particle size of not greater than about 30 microns.
  • the oxidizer particles comprise (a) at least one member selected from the group consisting of alkali metal nitrate and ammonium nitrate and (b) at least one member selected from the group consisting of alkali metal perchlorate and ammonium perchlorate.
  • the preferred alkali metal is potassium.
  • the solid pyrotechnic composition further comprises organic crystalline particles and optionally salts of organic crystalline particles.
  • the organic crystalline particles and the optional salts of organic crystalline particles preferably have a mean particle size of not greater than about 30 microns and preferably account for about 10 weight percent to about 60 weight percent of the total weight of the solid pyrotechnic composition.
  • the organic crystalline particles preferably comprise phenolphthalein.
  • a solid pyrotechnic composition comprising a boron/potassium nitrate substitute is provided for attaining the immediately above-mentioned object and other objects.
  • the composition comprises about 40 weight percent to about 90 weight percent oxidizer particles having a mean particle size of not greater than about 30 microns.
  • the oxidizer particles comprise at least one member selected from the group consisting of alkali metal perchlorate and ammonium perchlorate.
  • the perchlorate particles make up from about 20 weight percent to about 90 weight percent of the total weight of the composition, and more preferably 30 weight percent to 90 weight percent of the total weight of the composition.
  • the oxidizer particles may also comprise other materials, including at least one member selected from the group consisting of alkali metal nitrate and ammonium nitrate.
  • the preferred alkali metal for the perchlorate and nitrate is potassium.
  • the solid pyrotechnic composition further comprises organic crystalline particles and optionally salts of organic crystalline particles.
  • the organic crystalline particles and the optional salts of organic crystalline particles preferably have a mean particle size of not greater than 30 microns and preferably account for about 10 weight percent to about 60 weight percent of the total weight of the solid pyrotechnic composition.
  • the organic crystalline particles are preferably phenolphthalein.
  • the selection of the ingredients of these novel black powder and B/KNO3 substitute compositions can significantly reduce the production of harmful effluents derived from sulfur.
  • the invention can provide an improvement in the environmental impact and worker health risks encountered during firing and conducting post-fire clean-up operations of articles using the compositions.
  • the solid pyrotechnic composition according to presently preferred embodiments may possess excellent impact and thermal sensitivities, thereby reducing the incipient hazards of the igniter to detonation and premature ignition via response to stimuli such as impact, friction, heat, and/or electrostatic discharge.
  • the above-mentioned object and other objects are attained by a process in which an alkali metal hydroxide is combined with at least one organic crystalline compound to produce a solution comprising a salt of the organic crystalline compound.
  • the organic crystalline compound is preferably selected from the group consisting of phenolphthalein and a compound derived from reaction between a phenolic compound and phthalic anhydride.
  • the solution is then combined with at least one acid selected from the group consisting of nitric acid and perchloric acid.
  • the alkali metal hydroxide reacts with the nitric acid or perchloric acid to form alkali metal nitrate particles or alkali metal perchlorate particles, respectively.
  • the acid serves to convert the salt back to the organic crystalline compound, while reducing the particle size of the organic crystalline compound to not greater than about 30 microns.
  • Additional oxidizers particles having a mean particle size of not greater than about 30 microns may be added.
  • the additional oxidizer particles comprise a perchlorate salt and/or a nitrate salt.
  • the pyrotechnic composition may then be dried, if necessary or desired.
  • a black powder substitute pyrotechnic composition that comprises oxidizer particles and organic crystalline particles.
  • the oxidizer particles according to this embodiment constitute from about 40 weight percent to about 90 weight percent, more preferably 65 weight percent to 80 weight percent, of the total weight of the solid pyrotechnic composition.
  • the mean particle size of the oxidizer particles is not greater than about 30 microns, preferably is not greater than 20 microns, and more preferably is in a range of 5 microns to 20 microns.
  • the oxidizer particles of this embodiment comprise at least one nitrate salt.
  • the nitrate salt is preferably at least one member selected from the group consisting of alkali metal nitrate and ammonium nitrate.
  • alkali metal nitrates are potassium nitrate, cesium nitrate, rubidium nitrate, and ammonium nitrate, with potassium nitrate being preferred.
  • the oxidizer particles of this embodiment also comprise at least one perchlorate salt.
  • the perchlorate salt is preferably at least one member selected from the group consisting of potassium perchlorate and ammonium perchlorate, with potassium perchlorate being preferred.
  • the perchlorate salt can be instrumental in permitting the omission of sulfur from the pyrotechnic composition without sacrificing ballistic performance.
  • the perchlorate salt can decrease ignition delay of the pyrotechnic composition while increasing pressure rise. It is preferred that 0.5 weight percent to 30 weight percent of the total weight of the solid pyrotechnic composition consist the perchlorate salt. More preferably, 5 to 20 weight percent of the solid pyrotechnic composition consists of the perchlorate salt.
  • the organic crystalline particles of this embodiment account for about 10 weight percent to about 60 weight, more preferably 13 weight percent to 22 weight percent, of the total weight of the solid pyrotechnic composition. If a salt is present, it is preferred that at least 50 weight percent, more preferably at least 80 weight percent, and still more preferably at least 90 weight percent of the organic crystalline compound be present in a salt-free state. It is possible, and preferred, to use the organic crystalline alone, so that the solid pyrotechnic composition is free of any salts of organic crystalline compounds.
  • organic crystalline particles and its optional salts may have mean particle sizes as large as 100 microns, they preferably have a mean particle size of not greater than about 30 microns, more preferably not greater than 20 microns, still more preferably not greater than 15 microns, and still more preferably not greater than 10 microns.
  • the organic crystalline particles comprise at least one member selected from the group consisting of phenolphthalein and an organic crystalline compound derived from reaction between a phenolic compound and phthalic anhydride.
  • one or more of the 2-6 positions on the phenolic compound and/or one or more of the 2-5 positions on the phthalic anhydride compound can be substituted with functional groups such as -R, -NH 2 , -NR ⁇ , -NR ⁇ 2 , -N0 2 , -OR, and the like, in which R, R 1 , and R 2 are independently selected from, for example, alkyls and aryls.
  • the solid pyrotechnic composition of this invention is not limited to phenolphthalein and its derivatives. Instead, other organic crystalline compounds known in the art and those yet to be discovered may also be used. Representative organic crystalline compounds that may be of use with the present invention are described in U.S. Patent & Trademark Office document H72 to Wise, et al. and include fluorescein, 1,5- naphthalenediol, anthraflavic acid, terephthalic acid.
  • the solid pyrotechnic composition of this invention may optionally contain additional ingredients, including non-hygroscopic polymeric binders, for example.
  • suitable non-hygroscopic polymeric binders include those that uptake (i.e., absorb) less than 4% moisture at 75% RH (21.1°C (70°F)) over 24 hrs.
  • binders include: poly(vinyl acetate), poly(vinyl acetate- co-vinyl alcohol), nylon, poly(ethylene-co-vinyl acetate), polyethylene glycol, alkyl cellulose (e.g., ethyl cellulose), nitrocellulose, certain chain-extended oxetanes (e.g., polyBAMO), glycidyl azide polymer (GAP), and related polymers.
  • Suitable solvent may be used in the process for dissolving the binder and lowering viscosity during production.
  • ethyl acetate is a suitable solvent for poly(vinyl acetate).
  • water may be used to facilitate mixing.
  • the binders may be present in the composition in a concentration of not more than about 10 weight percent, preferably 3 weight percent to 6 weight percent.
  • the use of a non- hygroscopic binder and the organic crystalline compound lower the moisture uptake of the solid pyrotechnic composition of this invention.
  • the moisture uptake of the solid pyrotechnic composition is not greater than 0.3 weight percent, more preferably not greater than 0.25 weight percent, at 75 percent relative humidity and 21.1°C (70°F) over a period of 24 hours.
  • the black powder substitute (BPS) composition comprises 61.6 weight percent 15 micron potassium nitrate, 15 weight percent 20 micron potassium. perchlorate, 18.9 weight percent 6 micron phenolphthalein, and 4.5 weight percent 500,000 MW poly(vinyl acetate).
  • a B/KNO3 substitute pyrotechnic composition that comprises perchlorate salt oxidizer particles and organic crystalline particles.
  • Suitable perchlorate salts and organic crystalline particles for this embodiment of the invention can be selected from those described above and listed in connection with the black powder substitute composition.
  • boron/potassium nitrate burns at a relatively high theoretical flame temperature, preferably at least 2300K, and more preferably in a range of 2300K to 3000K. It is possible to obtain such high flame temperature by using a relatively high perchlorate salt loading, such as about 20 weight percent to about 90 weight percent, more preferably 30 weight percent to 90 weight percent, based on the total weight of the solid pyrotechnic composition. It has been found that perchlorate salts have a greater effect on raising theoretical flame temperature than other oxidizers such nitrate salts.
  • perchlorate salt in order to regulate theoretical flame temperature, lower loadings of perchlorate salt will be accompanied by high loadings of other oxidizers (e.g., nitrates) relative to organic crystalline compound and optional binder. On the other hand, higher loadings of perchlorate salt will be accompanied by low loadings of other oxidizers relative to organic crystalline compound and optional binder.
  • oxidizers e.g., nitrates
  • the binder is dissolved in a suitable solvent in a Hobart mixer, and the organic crystalline particles (e.g., phenolphthalein) are then added to the dissolved binder.
  • the oxidizer particles are added into the Hobart mixer.
  • the oxidizer particles may be added simultaneously or at different times from each other. If more than one types of oxidizer particles are used, the particles do not have to be premixed.
  • the ingredients are blended in the Hobart mixer as the solvent is removed, such as by vacuum or evaporation, until the material is prilled.
  • the prills are granulated to a suitable size, for example with a Stokes Granulator.
  • the granules are then dried under appropriate conditions, such as on aluminum trays in a convection oven at 135°F. After drying, additional granulation may be conducted to break up agglomerates.
  • This technique is merely exemplary. Many modifications may be made to this technique.
  • the binder may be pre-blended with the organic crystalline particles prior to adding the solvent. Similar conditions and steps may be used for processing with a twin- screw extruder.
  • the granules are to be pressed into pellets, blending of the granules with a suitable processing aid, such as calcium stearate, may be performed.
  • a suitable processing aid such as calcium stearate
  • the calcium stearate coating constitutes about 0.5 weight percent of the particles.
  • Pellets may be used as is, or may be further processed, such as by grinding, to make high density granules having comparable ballistics to granulated black powder.
  • an alkali metal hydroxide such as potassium hydroxide
  • at least one organic crystalline compound such as phenolphthalein or a phenolophthalein derivative
  • the solution is combined with nitric acid or perchloric acid, or if desired a combination of the acids.
  • the alkali metal hydroxide reacts with the nitric acid or perchloric acid to form alkali metal nitrate particles or alkali metal perchlorate particles, respectively.
  • the acid serves to convert the salt back to the organic crystalline compound, while preferably reducing the particle size of the organic crystalline compound to not greater than about 30 microns, preferably not greater than 20 microns.
  • Additional oxidizers particles having a mean particle size of not greater than about 30 microns may be added. This addition or combination step may be performed in-situ by reaction of the alkali metal hydroxide with the nitric or perchloric acid to form the oxidizer particles.
  • the oxidizer particles comprise a nitrate salt and/or a perchlorate salt.
  • the pyrotechnic composition may then be dried, if necessary or desired. By way of example and without limitation, drying may be conducted under vacuum or at atmospheric pressure, and may be conducted at room or elevated temperatures. Drying methods are well known in the art.
  • the suspended stream of particles is impinged by a small laser beam creating a diffraction pattern of light.
  • This diffraction pattern of light is converted into an energy distribution matrix which yields the various particle size properties such as intensity, distribution, mean diameter, cumulative volume, and so forth for the given sample.
  • the solid pyrotechnic compositions of this invention are useful for various applications, including, by way of example, as initiators, first fire compositions used with hot wires, gas generants, propellants, and the like.
  • the solid pyrotechnic compositions of this invention may be used, for example, in flares, rocket motors, and secondary restraint systems ("air bag devices") in vehicles.
  • Ballistic performance was determined by igniting a 2 g sample with a hot wire in a 45 cc-closed bomb. Humidity uptake data were obtained by placing approximately 3 g of sample in aluminum weigh dishes in a closed container above a saturated sodium chloride solution at 21.1°C (70°F). Ballistic performance data are found in Table 1.
  • Example 4 The same formulation as in Example 1 was scaled up to a 50 g size: In a 100 ml plastic vial, 9.45 g (18.9 weight percent) 6-micron phenolphthalein, 30.8 g (61.6 weight percent) 15-micron potassium nitrate, and 7.5 g (15 weight percent) 20-micron potassium perchlorate were dry blended for 1 min in a mini paint shaker. To these powders, 7.3 g of a 30.87% poly(vinyl acetate) in ethyl acetate (4.5 weight percent PVA dry weight) as well as 5.0 g of ethyl acetate were added. The sample was mixed, granulated and tested ballistically as in Example 1 and for humidity uptake as in Example 2.
  • Example 4 Example 4
  • Example three was repeated except for moisture uptake testing.
  • Example 1 Further 20-g samples of the black powder substitute were mixed, granulated, dried and tested ballistically as in Example 1 and tested for moisture uptake as in Example 2. These formulations had varying levels of 6-micron phenolphthalein, 20-micron potassium perchlorate and 15 micron potassium nitrate. The amount of ethyl acetate and poly (vinyl acetate) dissolved in ethyl acetate remained the same. The formulation and testing data are summarized in Table 1.
  • Formulations were also prepared in which sulfur was an ingredient in addition to the ingredients listed in Example 2.
  • the method of preparation varied such that the 70-micron phenolphthalein and the sulfur were pre-blended in a 125 ml plastic vial on the paint shaker in the presence of 0.635 cm (0.25 inch) diameter plastic beads before the blended material was added to the black powder substitute mix in a 20-g Nalgene vial.
  • Ballistic data should be compared to those for Example 2 in Table 1 since this formulation has phenolphthalein with a comparable particle size.
  • the inventive formulations had equivalent or superior ballistic properties to conventional black powder and conventional black powder substitute compositions.
  • the ballistic properties were especially good for Examples 1, 3- 5, 7, and 8, in which the total oxidizer concentration was present in a range of 65 and 80 weight percent and the phenolphthalein was present in a range of 13 to 22 weight percent.
  • Example 2 used relatively large phenolphthalein particles of 70 microns.
  • Examples 6 and 9 possessed more than 80 weight percent oxidizer.
  • Table 2 demonstrates the high moisture uptake that a crystalline salt of phenolphthalein has in comparison to phenolphthalein in its organic crystalline state.
  • the ratio of organic crystalline compound to salt has an inverse relationship to moisture uptake, i.e., as the ratio increased, the moisture uptake decreased.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Air Bags (AREA)

Abstract

La présente invention concerne une composition pyrotechnique solide qui présente des propriétés de température de combustion et de rendement balistique comparables à celles de la poudre noire, mais qui est de préférence formulée pour ne contenir ni charbon de bois ni soufre. Cette invention concerne également une composition pyrotechnique solide qui présente une température de combustion et un rendement balistique comparables à ceux du nitrate de potassium/bore et qui est de préférence dépourvue de bore.
EP02789146A 2001-01-12 2002-01-11 Compositions pyrotechniques solides absorbant peu l'humidite et procedes de production de ces dernieres Withdrawn EP1427683A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US26111101P 2001-01-12 2001-01-12
US261111P 2001-01-12
PCT/US2002/021566 WO2003022783A2 (fr) 2001-01-12 2002-01-11 Compositions pyrotechniques solides absorbant peu l'humidite et procedes de production de ces dernieres

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EP1427683A2 true EP1427683A2 (fr) 2004-06-16

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EP02789146A Withdrawn EP1427683A2 (fr) 2001-01-12 2002-01-11 Compositions pyrotechniques solides absorbant peu l'humidite et procedes de production de ces dernieres

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US (2) US20020148541A1 (fr)
EP (1) EP1427683A2 (fr)
JP (1) JP3981356B2 (fr)
AU (1) AU2002353766A1 (fr)
CA (1) CA2434730A1 (fr)
WO (1) WO2003022783A2 (fr)

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US20060042731A1 (en) 2006-03-02
WO2003022783A3 (fr) 2004-04-01
JP3981356B2 (ja) 2007-09-26
WO2003022783A2 (fr) 2003-03-20
AU2002353766A1 (en) 2003-03-24
CA2434730A1 (fr) 2003-03-20
JP2005506945A (ja) 2005-03-10
US20020148541A1 (en) 2002-10-17

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