EP0663896B1 - Powder precursor product - Google Patents
Powder precursor product Download PDFInfo
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- EP0663896B1 EP0663896B1 EP93922517A EP93922517A EP0663896B1 EP 0663896 B1 EP0663896 B1 EP 0663896B1 EP 93922517 A EP93922517 A EP 93922517A EP 93922517 A EP93922517 A EP 93922517A EP 0663896 B1 EP0663896 B1 EP 0663896B1
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- Prior art keywords
- nitrocellulose
- crystalline
- explosive
- explosive substance
- crystalline explosive
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
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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
- C06B21/0033—Shaping the mixture
- C06B21/0066—Shaping the mixture by granulation, e.g. flaking
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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
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
Definitions
- the invention relates to a method for producing a precursor for powder or explosive, which consists essentially of nitrocellulose and at least one crystalline explosive, in particular hexogen, and in which the crystalline explosive is combined with the nitrocellulose in the aqueous phase. Furthermore, the invention relates to a precursor for powder or explosive, which essentially consists of nitrocellulose and at least one crystalline explosive, which was combined with the nitrocellulose in the aqueous phase.
- a powder raw mass is usually first produced, which essentially consists of nitrocellulose and an explosive oil, for example diglycol dinitrate. Hexogen is then introduced into this raw powder mass as a further working step.
- a method for producing a rocket fuel is already known from US Pat. No. 3,702,272, in which a nitrocellulose lacquer is stirred into the aqueous suspension of a crystalline explosive, for example hexogen.
- the crystalline explosive in the suspension should have a grain size of 0.1 to 150 ⁇ m, preferably 1 to 30 ⁇ m.
- the nitrocellulose lacquer added to the suspension is obtained beforehand by dissolving nitrocellulose in an organic solvent.
- the known method has been proposed primarily in terms of the safe handling of the very sensitive crystalline explosive during manufacture.
- An explosive is also already known from US Pat. No. 3,311,513, which consists of a nitramine as crystalline component, nitrocellulose and a plasticizer for the nitrocellulose.
- the nitramine should preferably be one Particle size between 1 and 75 microns.
- the nitramine is first introduced into the plasticizer and then the nitrocellulose.
- an explosive consisting of a nitramine and a highly viscous, plasticized nitrocellulose is known from US Pat. No. 401,472, in which the particle size of the crystalline component should be less than 25 ⁇ m.
- the object of the invention is to propose a method in which the crystalline explosive is distributed particularly uniformly in the raw mass of the preliminary product.
- the process according to the invention allows the crystalline explosive to be distributed particularly uniformly in the raw mass of the preliminary product. In addition to the very homogeneous distribution, it is also achieved that the crystalline explosive component is particularly firmly connected to the nitrocellulose and thus has a high abrasion resistance.
- the finely crystalline explosive with the specified average particle diameter can be drawn onto the fibers of the nitrocellulose.
- the crystalline explosive and the nitrocellulose are each stirred in the aqueous phase in a separate container.
- the crystalline explosive can advantageously be stirred up in surfactant water (for example with a surfactant concentration of 0.1%).
- the components that are stirred up are then brought together with stirring. As a result, particularly good mixing between the crystalline explosive and the nitrocellulose is achieved.
- An explosive oil in particular diglycol dinitrate, can advantageously be added and preferably stirred after the nitrocellulose and crystalline explosive have been brought together. The resulting gelatinization of the nitrocellulose results in an additional binding of the crystalline explosive to the nitrocellulose.
- an explosive oil in particular diglycol dinitrate, can be combined with the nitrocellulose and then the crystalline explosive can then be added.
- the raw mass containing the crystalline explosive is separated from the liquid, a centrifugation method preferably being used. It has been shown that after drying the filter cake there is no increased formation of dust under mechanical stress compared to known powder raw materials which have no crystalline explosive component. This makes it clear that the crystalline explosive is particularly intimately involved.
- a propeller stirrer can be used for stirring.
- the method according to the invention can also be used with a crystalline explosive which has a wax additive.
- a wax additive serve to desensitize the highly explosive crystalline explosive.
- the nitrocellulose used advantageously has a nitrogen content of about 12.6%.
- the stirring in water takes place with little turbulence.
- At least one further explosive in particular nitroguanidine, can be added to the preliminary product.
- the further explosive is again added in suspension in accordance with the primary explosive.
- the crystalline explosive is particularly evenly distributed with respect to the nitrocellulose and firmly integrated into it.
- the new intermediate product has very uniform properties and a particularly high abrasion resistance.
- crystalline explosives, in particular hexogen, with a wax content can also be used.
- the preliminary product advantageously contains an explosive oil, in particular diglycol dinitrate.
- the process described below is intended to produce a raw material for a propellant charge powder which contains about 55% nitrocellulose, 34% diglycol dinitrate and about 11% crystalline explosive.
- the nitrocellulose used has a nitrogen content of 12.6% and a water content of 33.3%.
- the moist crystalline explosive is first stirred intimately in a first stirred container with a small amount of surfactant water (surfactant concentration 0.1%) and then stirred up with milk cream with the further addition of water. If the turbulence is low, the nitrocellulose is also stirred in water in a second stirred tank. In this slurry, the contents of the first stirred tank are added in portions with continued stirring. Then continue stirring for about 10 minutes. Subsequently, diglycol dinitrate is added in a thin stream with moderate stirring and stirring is continued for about 20 minutes. The raw material containing hexogen is then centrifuged off.
- surfactant water surfactant concentration 0.15%
- the still moist raw material of the preliminary product is obtained as a centrifugate.
- this raw material containing the crystalline explosive cannot be distinguished from conventional raw materials which do not contain any crystalline explosive with regard to the mechanical and safety properties.
- the powder precursor can be easily transported when moist with water and can be supplemented with the addition of another explosive component, for example nitroguanidine.
- another explosive component for example nitroguanidine.
- wax-containing crystalline explosives in particular wax-containing hexogen, can also be used.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Cosmetics (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Herstellung eines vorproduktes für Pulver oder Sprengstoff, das im wesentlichen aus Nitrocellulose und mindestens einem kristallinen Explosivstoff, insbesondere Hexogen, besteht, und bei dem der kristalline Explosivstoff in wässriger Phase mit der Nitrocellulose zusammengeführt wird. Weiterhin bezieht sich die Erfindung auf ein Vorprodukt für Pulver oder Sprengstoff, das im wesentlichen aus Nitrocellulose und mindestens einem kristallinen Explosivstoff besteht, der mit der Nitrocellulose in wässriger Phase zusammengeführt wurde.The invention relates to a method for producing a precursor for powder or explosive, which consists essentially of nitrocellulose and at least one crystalline explosive, in particular hexogen, and in which the crystalline explosive is combined with the nitrocellulose in the aqueous phase. Furthermore, the invention relates to a precursor for powder or explosive, which essentially consists of nitrocellulose and at least one crystalline explosive, which was combined with the nitrocellulose in the aqueous phase.
Bei der Herstellung von Treibladungspulvern mit Hexogen wird üblicherweise zunächst eine Pulverrohmasse hergestellt, die im wesentlichen aus Nitrocellulose und einem Sprengöl, beispielsweise Diglykoldinitrat, besteht. In diese Pulverrohmasse wird dann als weiterer Arbeitsgang Hexogen eingebracht.In the production of propellant charge powders with hexogen, a powder raw mass is usually first produced, which essentially consists of nitrocellulose and an explosive oil, for example diglycol dinitrate. Hexogen is then introduced into this raw powder mass as a further working step.
Aus der US-PS 3 702 272 ist bereits ein Verfahren zur Herstellung eines Raketentreibstoffes bekannt, bei welchem in die wässrige Suspension eines kristallinen Explosivstoffes, zum Beispiel Hexogen, ein Nitrocellulose-Lack eingerührt wird. Der kristalline Explosivstoff in der Suspension soll eine Kornfeinheit von 0,1 bis 150 µm, vorzugsweise 1 bis 30 µm haben. Der der Suspension zugesetzte Nitrocellulose-Lack wird zuvor dadurch erhalten, daß Nitrocellulose in einem organischen Lösungsmittel gelöst wird. Das bekannte Verfahren ist in erster Linie unter dem Aspekt der sicheren Handhabung des sehr empfindlichen kristallinen Explosivstoffes bei der Herstellung vorgeschlagen worden.A method for producing a rocket fuel is already known from US Pat. No. 3,702,272, in which a nitrocellulose lacquer is stirred into the aqueous suspension of a crystalline explosive, for example hexogen. The crystalline explosive in the suspension should have a grain size of 0.1 to 150 µm, preferably 1 to 30 µm. The nitrocellulose lacquer added to the suspension is obtained beforehand by dissolving nitrocellulose in an organic solvent. The known method has been proposed primarily in terms of the safe handling of the very sensitive crystalline explosive during manufacture.
Aus der US-PS 3 311 513 ist ebenfalls bereits ein Explosivstoff bekannt, der aus einem Nitramin als kristalline Komponente, Nitrocellulose und einem Plastifiziermittel für die Nitrocellulose besteht. Das Nitramin soll bevorzugt eine Teilchengröße zwischen 1 und 75 µm haben. Bei der Herstellung wird zunächst das Nitramin in das Plastifiziermittel eingebracht und anschließend die Nitrocellulose. In ähnlicher Weise ist aus der US-PS 401 472 ein Explosivstoff aus einem Nitramin und einer hochviskosen, plastifizierten Nitrocellulose bekannt, bei welchem die Teilchengröße der kristallinen Komponente kleiner als 25 µm sein soll.An explosive is also already known from US Pat. No. 3,311,513, which consists of a nitramine as crystalline component, nitrocellulose and a plasticizer for the nitrocellulose. The nitramine should preferably be one Particle size between 1 and 75 microns. During production, the nitramine is first introduced into the plasticizer and then the nitrocellulose. Similarly, an explosive consisting of a nitramine and a highly viscous, plasticized nitrocellulose is known from US Pat. No. 401,472, in which the particle size of the crystalline component should be less than 25 μm.
Ausgehend hiervon liegt der Erfindung die Aufgabe zugrunde, ein Verfahren vorzuschlagen, bei dem der kristalline Explosivstoff besonders gleichmäßig in der Rohmasse des Vorproduktes verteilt ist.Proceeding from this, the object of the invention is to propose a method in which the crystalline explosive is distributed particularly uniformly in the raw mass of the preliminary product.
Zur Lösung dieser Aufgabe wird bei einem Verfahren der eingangs genannten Art vorgeschlagen, daß der kristalline Explosivstoff in feinkristalliner Form mit einem mittleren Partikeldurchmesser d₅₀ = 2 bis 8 µm vorliegt, daß der kristalline Explosivstoff und die Nitrocellulose voneinander getrennt, jeweils in wässriger Phase aufgerührt werden und daß der kristalline Explosivstoff und die Nitrocellulose unter Rühren zusammengeführt werden.To solve this problem it is proposed in a method of the type mentioned that the crystalline explosive is in fine crystalline form with an average particle diameter d₅₀ = 2 to 8 microns, that the crystalline explosive and the nitrocellulose are separated from one another, are each stirred in the aqueous phase and that the crystalline explosive and the nitrocellulose are brought together with stirring.
Durch das erfindungsgemäße Verfahren kann der kristalline Explosivstoff besonders gleichmäßig in der Rohmasse des Vorproduktes verteilt werden. Neben der sehr homogenen Verteilung wird weiterhin erreicht, daß die kristalline Explosivstoffkomponente besonders fest mit der Nitrocellulose verbunden ist und somit eine hohe Abriebfestigkeit aufweist. Hierbei wird bei dem erfindungsgemäßen Verfahren von der Erkenntnis ausgegangen, daß sich der feinstkristalline Explosivstoff mit dem angegebenen mittleren Partikeldurchmesser auf die Fasern der Nitrocellulose aufziehen läßt. Zunächst wird der kristalline Explosivstoff und die Nitrocellulose jeweils in wässriger Phase in einem separaten Behältnis aufgerührt. Hierbei kann vorteilhaft der kristalline Explosivstoff in Tensidwasser (beispielsweise mit einer Tensidkonzentration von 0,1 %) aufgerührt werden. Anschließend werden die jeweils aufgerührten Komponenten unter Rühreintrag zusammengeführt. Hierdurch wird eine besonders gute Vermischung zwischen dem kristallinen Explosivstoff und der Nitrocellulose erreicht.The process according to the invention allows the crystalline explosive to be distributed particularly uniformly in the raw mass of the preliminary product. In addition to the very homogeneous distribution, it is also achieved that the crystalline explosive component is particularly firmly connected to the nitrocellulose and thus has a high abrasion resistance. In the process according to the invention, it is assumed that the finely crystalline explosive with the specified average particle diameter can be drawn onto the fibers of the nitrocellulose. First, the crystalline explosive and the nitrocellulose are each stirred in the aqueous phase in a separate container. The crystalline explosive can advantageously be stirred up in surfactant water (for example with a surfactant concentration of 0.1%). The components that are stirred up are then brought together with stirring. As a result, particularly good mixing between the crystalline explosive and the nitrocellulose is achieved.
Vorteilhaft kann ein Sprengöl, insbesondere Diglykoldinitrat, nach dem Zusammenführen von Nitrocellulose und kristallinem Explosivstoff zugegeben und vorzugsweise verrührt werden. Die hierdurch bewirkte Gelatinierung der Nitrocellulose hat eine zusätzliche Bindung des kristallinen Explosivstoffes an der Nitrocellulose zur Folge. Alternativ kann ein Sprengöl, insbesondere Diglykoldinitrat, mit der Nitrocellulose zusammengeführt werden und nachfolgend kann dann der kristalline Explosivstoff zugegeben werden.An explosive oil, in particular diglycol dinitrate, can advantageously be added and preferably stirred after the nitrocellulose and crystalline explosive have been brought together. The resulting gelatinization of the nitrocellulose results in an additional binding of the crystalline explosive to the nitrocellulose. Alternatively, an explosive oil, in particular diglycol dinitrate, can be combined with the nitrocellulose and then the crystalline explosive can then be added.
In weiterer Ausgestaltung wird die den kristallinen Explosivstoff enthaltende Rohmasse von der Flüssigkeit abgetrennt, wobei vorzugsweise ein Zentrifugationsverfahren eingesetzt wird. Es hat sich gezeigt, daß nach Trocknung des Filterkuchens keine vermehrte Staubbildung bei mechanischer Beanspruchung gegenüber bekannten Pulverrohmassen auftritt, die keine kristalline Explosivstoffkomponente aufweisen. Hierdurch wird deutlich, daß der kristalline Explosivstoff besonders innig eingebunden ist.In a further embodiment, the raw mass containing the crystalline explosive is separated from the liquid, a centrifugation method preferably being used. It has been shown that after drying the filter cake there is no increased formation of dust under mechanical stress compared to known powder raw materials which have no crystalline explosive component. This makes it clear that the crystalline explosive is particularly intimately involved.
Bei einer vorteilhaften Ausgestaltung wird eine Mischung aus Hexogen und einem geringen Oktogenanteil, die einen mittleren Partikeldurchmesser d₅₀ = 5 bis 7 µm aufweist, zunächst mit einem verdünnten Tensidwasser verrührt und nachfolgend unter Wasserzugabe milchsahnig aufgerührt. Zum Aufrühren kann beispielsweise ein Propellerrührer zum Einsatz kommen.In an advantageous embodiment, a mixture of hexogen and a small amount of octogen, which has an average particle diameter d₅₀ = 5 to 7 μm, is first stirred with a dilute surfactant water and then stirred with the addition of milk creamy milk. For example, a propeller stirrer can be used for stirring.
Das erfindungsgemäße Verfahren ist auch bei einem kristallinen Explosivstoff einsetzbar, der einen Wachszusatz aufweist. Derartige Wachszusätze dienen der Phlegmatisierungs des hochbrisanten kristallinen Explosivstoffes.The method according to the invention can also be used with a crystalline explosive which has a wax additive. Such wax additives serve to desensitize the highly explosive crystalline explosive.
Die zum Einsatz kommende Nitrocellulose weist vorteilhaft einen Stickstoffgehalt von etwa 12,6% auf. Das Aufrühren in Wasser erfolgt unter geringer Turbulenz.The nitrocellulose used advantageously has a nitrogen content of about 12.6%. The stirring in water takes place with little turbulence.
Dem Vorprodukt kann mindestens ein weiterer Explosivstoff, insbesondere Nitroguanidin, zugesetzt werden. Hierbei wird der weitere Explosivstoff wiederum entsprechend dem primären Explosivstoff in Suspension aufgerührt zugegeben.At least one further explosive, in particular nitroguanidine, can be added to the preliminary product. In this case, the further explosive is again added in suspension in accordance with the primary explosive.
Weiterhin wird ein Vorprodukt für Pulver oder Sprengstoff beansprucht, das im wesentlichen aus Nitrocellulose und mindestens einem kristallinen Explosivstoff besteht, der in feinkristalliner Form mit einem mittleren Partikeldurchmesser von d₅₀ = 2 bis 8 µm vorliegt, wobei der kristalline Explosivstoff und die Nitrocellulose - nach getrenntem Aufrühren jeweils in wässriger Phase - unter Rühren zusammengeführt sind. Dadurch ist der kristalline Explosivstoff besonders gleichmäßig gegenüber der Nitrocellulose verteilt und in diese fest eingebunden. Das neue Vorprodukt hat sehr gleichmäßige Eigenschaften und eine besonders hohe Abriebfestigkeit. Außerdem können auch kristalline Explosivstoffe, insbesondere Hexogen, mit einem Wachsgehalt eingesetzt werden. Vorteilhafterweise enthält das Vorprodukt ein Sprengöl, insbesondere Diglykoldinitrat.Furthermore, a precursor for powder or explosive is claimed, which consists essentially of nitrocellulose and at least one crystalline explosive, which is in fine crystalline form with an average particle diameter of d₅₀ = 2 to 8 microns, the crystalline explosive and the nitrocellulose - after separate stirring each in the aqueous phase - are brought together with stirring. As a result, the crystalline explosive is particularly evenly distributed with respect to the nitrocellulose and firmly integrated into it. The new intermediate product has very uniform properties and a particularly high abrasion resistance. In addition, crystalline explosives, in particular hexogen, with a wax content can also be used. The preliminary product advantageously contains an explosive oil, in particular diglycol dinitrate.
Nachfolgend soll die vorliegende Erfindung anhand eines Beispiels näher erläutert werden.The present invention is to be explained in more detail below using an example.
Mit dem nachfolgend beschriebenen Verfahren soll eine Vorprodukt-Rohmasse für ein Treibladungspulver hergestellt werden, die etwa 55% Nitrocellulose, 34% Diglykoldinitrat und etwa 11% kristallinen Explosivstoff enthält. Der kristalline Explosivstoff ist eine Mischung aus Hexogen mit etwa 6% Oktogen, die einen mittleren Partikeldurchmesser d₅₀ = 6,2 µm und einen Wassergehalt von 13,3 % aufweist. Die verwendete Nitrocellulose besitzt einen Stickstoffgehalt von 12,6 % und einen Wassergehalt von 33,3%.The process described below is intended to produce a raw material for a propellant charge powder which contains about 55% nitrocellulose, 34% diglycol dinitrate and about 11% crystalline explosive. The crystalline explosive is a mixture of hexogen with about 6% octogen, which has an average particle diameter d₅₀ = 6.2 µm and a water content of 13.3%. The nitrocellulose used has a nitrogen content of 12.6% and a water content of 33.3%.
Der feuchte kristalline Explosivstoff wird in einem ersten Rührbehälter zunächst mit einer geringen Tensidwassermenge (Tensidkonzentration 0,1 %) innig verrührt und anschließend unter weiterer Zugabe von Wasser milchsahnig aufgerührt. In einem zweiten Rührbehälter wird bei geringer Turbulenz die Nitrocellulose ebenfalls in Wasser aufgerührt. In dieser Aufschlemmung wird unter fortgesetztem Rühren der Inhalt des ersten Rührbehälters portionsweise eingetragen. Anschließend wird für etwa 10 Minuten weitergerührt. Nachfolgend wird Diglykoldinitrat in dünnem Strahl unter mäßigem Rühren zugegeben und etwa 20 Minuten nachgerührt. Die hexogenhaltige Rohmasse wird nachfolgend abzentrifugiert.The moist crystalline explosive is first stirred intimately in a first stirred container with a small amount of surfactant water (surfactant concentration 0.1%) and then stirred up with milk cream with the further addition of water. If the turbulence is low, the nitrocellulose is also stirred in water in a second stirred tank. In this slurry, the contents of the first stirred tank are added in portions with continued stirring. Then continue stirring for about 10 minutes. Subsequently, diglycol dinitrate is added in a thin stream with moderate stirring and stirring is continued for about 20 minutes. The raw material containing hexogen is then centrifuged off.
Als Zentrifugat wird die noch feuchte Vorprodukt-Rohmasse erhalten. Bei Versuchen wurde festgestellt, daß diese den kristallinen Explosivstoff enthaltende Rohmasse von herkömmlichen Rohmassen, die keinen kristallinen Explosivstoff enthalten, hinsichtlich der mechanischen und sicherheitstechnischen Eigenschaften nicht zu unterscheiden ist. Auch wurde nach Trocknung des Zentrifugats keine vermehrte Staubbildung bei mechanischer Beanspruchung festgestellt.The still moist raw material of the preliminary product is obtained as a centrifugate. Experiments have shown that this raw material containing the crystalline explosive cannot be distinguished from conventional raw materials which do not contain any crystalline explosive with regard to the mechanical and safety properties. Even after drying the centrifugate, no increased dust formation was found under mechanical stress.
Die Reibempfindlichkeit dieser Hexogen-Rohmasse beträgt in trockenem Zustand 21,6 kp = 216 N Stiftbelastung und die Schlagempfindlichkeit liegt bei 0,5 kpm = 5 Nm. Diese Werte wurden auch bei den bisherigen Rohmassen festgestellt, die kein Hexogen enthielten.The friction sensitivity of this hexogen raw mass when dry is 21.6 kp = 216 N pin load and the impact sensitivity is 0.5 kpm = 5 Nm. These values were also found in the previous raw materials that did not contain any hexogen.
Das Pulver-Vorprodukt ist wasserfeucht gut transportfähig und kann unter Zugabe einer weiteren Explosivstoffkomponente, beispielsweise Nitroguanidin, ergänzt werden.The powder precursor can be easily transported when moist with water and can be supplemented with the addition of another explosive component, for example nitroguanidine.
Es hat sich gezeigt, daß auch wachshaltige kristalline Explosivstoffe, insbesondere wachshaltiges Hexogen, zum Einsatz kommen können.It has been shown that wax-containing crystalline explosives, in particular wax-containing hexogen, can also be used.
Claims (11)
- Process for the preparation of a powder or explosive intermediate which comprises substantially nitrocellulose and at least one crystalline explosive substance, in particular hexogen, and in which the crystalline explosive substance is brought together in aqueous phase with the nitrocellulose, characterised in that the crystalline explosive substance is present in finely crystalline form having an average particle diameter of d₅₀ = 2 to 8 µm, that the crystalline explosive substance and the nitrocellulose are each slurried in aqueous phase separately from one another, and that the crystalline explosive substance and the nitrocellulose are brought together, with stirring.
- Process according to Claim 1, characterised in that an explosive oil, in particular diglycol dinitrate, is added after the nitrocellulose and the crystalline explosive substance have been brought together, and is preferably stirred up.
- Process according to Claim 1, characterised in that an explosive oil, in particular diglycol dinitrate, is brought together with the nitrocellulose, and the crystalline explosive substance is added subsequently.
- Process according to one of Claims 1 to 3, characterised in that the intermediate containing the crystalline explosive substance is separated from the liquid, with a centrifuging process being preferably utilised.
- Process according to one of Claims 1 to 4, characterised in that a mixture of hexogen and a small proportion of octogen, which exhibits an average particle diameter d₅₀ = 5 to 7 µm, is first stirred up with a dilute surfactant water and is slurried subsequently, with the addition of water until thinly creamy.
- Process according to one of Claims 1 to 5, characterised in that the crystalline explosive substance may exhibit added wax.
- Process according to one of Claims 1 to 6, characterised in that the nitrocellulose exhibits a nitrogen content of approximately 12.6% and is slurried in water, with slight turbulence.
- Process according to one of Claims 3 to 7, characterised in that there is added to the intermediate at least one further explosive substance, in particular nitroguanidine.
- Powder or explosive intermediate which comprises substantially nitrocellulose and at least one crystalline explosive substance, in particular hexogen, which is brought together in aqueous phase with the nitrocellulose, characterised in that the crystalline explosive substance is present in finely crystalline form having an average particle diameter of d₅₀ = 2 to 8 µm, and that the crystalline explosive substance and the nitrocellulose are brought together, with stirring, after each being slurried separately in aqueous phase.
- Intermediate according to Claim 9, characterised in that the crystalline explosive substance, in particular hexogen, exhibits a wax content.
- Intermediate according to Claim 9 or 10, characterised in that the intermediate contains an explosive oil, in particular diglycol dinitrate.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4233629A DE4233629C2 (en) | 1992-10-06 | 1992-10-06 | Process for producing a powder precursor and powder precursor |
| DE4233629 | 1992-10-06 | ||
| PCT/EP1993/002722 WO1994007813A1 (en) | 1992-10-06 | 1993-10-05 | Powder precursor product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0663896A1 EP0663896A1 (en) | 1995-07-26 |
| EP0663896B1 true EP0663896B1 (en) | 1996-03-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP93922517A Expired - Lifetime EP0663896B1 (en) | 1992-10-06 | 1993-10-05 | Powder precursor product |
Country Status (7)
| Country | Link |
|---|---|
| EP (1) | EP0663896B1 (en) |
| AT (1) | ATE135674T1 (en) |
| AU (1) | AU5149293A (en) |
| DE (1) | DE4233629C2 (en) |
| ES (1) | ES2086966T3 (en) |
| GR (1) | GR3020086T3 (en) |
| WO (1) | WO1994007813A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441550C (en) * | 1996-07-22 | 2008-12-10 | 大赛璐化学工业株式会社 | Gas generant for air bag |
| GB9913262D0 (en) * | 1999-06-09 | 2002-08-21 | Royal Ordnance Plc | Desensitation of energetic materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1025694A (en) * | 1962-02-19 | 1966-04-14 | North American Aviation Inc | Polymer coating of solid particles |
| US3235420A (en) * | 1962-05-04 | 1966-02-15 | Du Pont | Process of making homogeneous particles comprising nitrocellulose mixtures |
| US3329743A (en) * | 1963-05-15 | 1967-07-04 | Olin Mathieson | Lacquer process for preparing small diameter nitrocellulose particles |
| US3702272A (en) * | 1964-01-10 | 1972-11-07 | Olin Mathieson | Spherical rocket propellant casting granules and method of preparation |
| US3311513A (en) * | 1965-03-05 | 1967-03-28 | Du Pont | Nitramine, nitrocellulose explosive with ester plasticizer |
| DE2316538C3 (en) * | 1973-04-03 | 1982-05-06 | Dynamit Nobel Ag, 5210 Troisdorf | Process for the production of Gudol powder |
| DE2461646C2 (en) * | 1974-12-27 | 1984-01-05 | Dynamit Nobel Ag, 5210 Troisdorf | Process for the production of propellant charge powders |
| US4014720A (en) * | 1975-10-28 | 1977-03-29 | The United States Of America As Represented By The Secretary Of The Army | Flexible explosive composition comprising particulate RDX, HMX, or PETN and a high viscosity introcellulose binder plasticized with TEGDN |
| NO144666C (en) * | 1980-02-29 | 1981-10-14 | Dyno Industrier As | PROCEDURE FOR PREPARING ALUMINUM-CONTAINING HIGH-ENERGY EXPLOSIVE MIXTURES |
| CH643804A5 (en) * | 1980-07-24 | 1984-06-29 | Oerlikon Buehrle Ag | Explosive and process for its manufacture |
| DE3532525A1 (en) * | 1985-09-12 | 1987-03-19 | Fraunhofer Ges Forschung | THREE-BASED POWDER CHARGING POWDER AND METHOD FOR THE PRODUCTION THEREOF |
-
1992
- 1992-10-06 DE DE4233629A patent/DE4233629C2/en not_active Expired - Fee Related
-
1993
- 1993-10-05 EP EP93922517A patent/EP0663896B1/en not_active Expired - Lifetime
- 1993-10-05 AT AT93922517T patent/ATE135674T1/en not_active IP Right Cessation
- 1993-10-05 ES ES93922517T patent/ES2086966T3/en not_active Expired - Lifetime
- 1993-10-05 WO PCT/EP1993/002722 patent/WO1994007813A1/en active IP Right Grant
- 1993-10-05 AU AU51492/93A patent/AU5149293A/en not_active Abandoned
-
1996
- 1996-05-30 GR GR960401442T patent/GR3020086T3/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| ES2086966T3 (en) | 1996-07-01 |
| AU5149293A (en) | 1994-04-26 |
| EP0663896A1 (en) | 1995-07-26 |
| GR3020086T3 (en) | 1996-08-31 |
| DE4233629A1 (en) | 1994-04-07 |
| DE4233629C2 (en) | 1994-09-15 |
| ATE135674T1 (en) | 1996-04-15 |
| WO1994007813A1 (en) | 1994-04-14 |
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