EP1505047A2 - Use of a microjet reactor for manufacturing a primary explosive - Google Patents
Use of a microjet reactor for manufacturing a primary explosive Download PDFInfo
- Publication number
- EP1505047A2 EP1505047A2 EP04017847A EP04017847A EP1505047A2 EP 1505047 A2 EP1505047 A2 EP 1505047A2 EP 04017847 A EP04017847 A EP 04017847A EP 04017847 A EP04017847 A EP 04017847A EP 1505047 A2 EP1505047 A2 EP 1505047A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- reactor
- use according
- explosive
- production
- microjet
- 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- Withdrawn
Links
- 239000002360 explosive Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 150000001540 azides Chemical class 0.000 claims description 2
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 2
- MHVVRZIRWITSIP-UHFFFAOYSA-L lead(2+);2,4,6-trinitrophenolate Chemical compound [Pb+2].[O-]C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O.[O-]C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O MHVVRZIRWITSIP-UHFFFAOYSA-L 0.000 claims description 2
- VVOUQFXJSCDIAO-UHFFFAOYSA-L lead(2+);dinitrite Chemical compound [Pb+2].[O-]N=O.[O-]N=O VVOUQFXJSCDIAO-UHFFFAOYSA-L 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000037452 priming Effects 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
- C06C7/00—Non-electric detonators; Blasting caps; Primers
-
- 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
- C06B21/0008—Compounding the ingredient
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B41/00—Compositions containing a nitrated metallo-organic compound
Definitions
- the invention relates to the use of a microjet reactor for the production of initial explosive.
- the object of the invention is to overcome the disadvantages of the prior art overcome and create a process for the production of initial explosive in particular very small crystals (for example in the range from 0.5 to 30 ⁇ m, preferably from 1 to 20 .mu.m, particularly preferably from 1 to 10 .mu.m), wherein the crystal size obtained by setting process parameters largely controllable and where in each case a narrow and defined grain spectrum should be adjustable.
- very small crystals for example in the range from 0.5 to 30 ⁇ m, preferably from 1 to 20 .mu.m, particularly preferably from 1 to 10 .mu.m
- microjet reactor for the Production of initial explosive, wherein the starting solutions for Explosives production in the microjet reactor through one nozzle at a time from a reactor housing enclosed reactor space on a Common collision point to be injected via an opening in the Reactor space, a gas is introduced and the resulting Initial explosive crystals along with the liquid and excess gas be removed through a further opening from the reactor housing.
- One Microjet reactor is e.g. described in WO 00/61275, wherein on the entire disclosure content of this document here express reference is taken.
- the size of the resulting explosive crystals in the precipitation can be through Varying the operating parameters reproducibly control. This can be the Diameter of the reactant supplying nozzles, the pump pressure, the Temperatures and concentrations of the starting solutions and the amount of Auxiliary gases are varied.
- the nozzle diameter is preferably 10 to 1000 microns, more preferably 50 to 500 microns and most preferably 50 to 100 ⁇ m.
- the total flow rate is preferably 10 to 1000 ml / minute, more preferably 50 to 500 ml / minute.
- the use according to the invention makes it possible to prefer the following Make initial explosives: potassium dinitrobenzofuroxanate, lead azide, lead picrate, Leadrinitic resorcinate and cesium dinitrobenzofuroxanate.
- Another advantage of the use according to the invention is that due to the defined crystal size of the initial explosive one fractionated (and dangerous) screening can be omitted.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
Description
Die Erfindung betrifft die Verwendung eines Mikrojetreaktors für die Herstellung von Initialsprengstoff.The invention relates to the use of a microjet reactor for the production of initial explosive.
Viele Initialsprengstoffe werden hergestellt, indem mindestens zwei Ausgangslösungen gemischt werden und der Sprengstoff aus dieser Mischung in kristalliner Form ausfällt. Dabei wird versucht, durch Wahl der Reaktionsparameter (Temperatur, Bewegung der Mischung) bestimmte, reproduzierbare Kristallgrößen bei der Fällung zu erhalten. Dies gestaltet sich jedoch problematisch, da es schwierig ist, die Temperatur und die Bewegungsführung eines Fällbades im großen Maßstab zu steuern. Innerhalb des Fällbehälters stellen sich Temperaturgradienten ein, und durch Rührbewegungen wird die Kristallisation zusätzlich beeinflusst. Oftmals wird nach einer festgelegten Fälldauer die Flüssigkeit abgelassen und das kristalline Material abgefiltert und fraktioniert gesiebt. Die Möglichkeiten, reproduzierbar eine bestimmte Korngrößenverteilung zu erhalten, sind mit diesem Fällverfahren sehr begrenzt. In der Regel liegen die erhaltenen Korngrößenverteilungen in einem Bereich von bis zu zwei Zehnerpotenzen.Many initial explosives are made by at least two Starting solutions are mixed and the explosives from this mixture in crystalline form fails. An attempt is made by choosing the Reaction parameter (temperature, movement of the mixture) determined to obtain reproducible crystal sizes in the precipitation. This is happening However, it is problematic because it is difficult to control the temperature and the Control the movement of a precipitation bath on a large scale. Within of the precipitation tank, temperature gradients set, and by Stirring movements, the crystallization is additionally influenced. Often it will after Drained the liquid and the crystalline Material filtered off and fractionated sieved. The possibilities, reproducible to obtain a certain particle size distribution, are with this precipitation method very limited. In general, the grain size distributions obtained are in a range of up to two powers of ten.
Für Anzünder im Kraftfahrzeugsicherheitsbereich werden Initialzündstoffe, bzw. Initialsprengstoffe benötigt, die sehr kleine und reproduzierbare Kristallabmessungen (typische Größen von < 30 µm) aufweisen, damit eine gute thermische Kopplung zwischen den elektrischen Heizwiderständen und den Kristallen erfolgen kann. Auch bei anderen Anwendungen von Initialsprengstoffen ist es erwünscht, dass viele kleine Kristalle Kontakt zu dem jeweiligen Zündwiderstand haben.For lighters in the automotive safety area are initial igniters, or Initial explosives needed that are very small and reproducible Crystal dimensions (typical sizes of <30 microns), thus a good thermal coupling between the electrical heating resistors and the Crystals can be made. Also with other applications of Initial explosives, it is desirable that many small crystals make contact with the have respective ignition resistance.
Aufgabe der Erfindung ist es, die Nachteile des Standes der Technik zu überwinden und ein Verfahren zur Herstellung von Initialsprengstoff zu schaffen, das insbesondere zu sehr kleinen Kristallen (z.B. im Bereich von 0,5 bis 30 µm, bevorzugt von 1 bis 20 µm, besonders bevorzugt von 1 bis 10 µm) führt, wobei die erhaltene Kristallgröße durch Einstellen von Verfahrensparametern weitgehend steuerbar und wobei jeweils ein enges und definiertes Kornspektrum einstellbar sein soll.The object of the invention is to overcome the disadvantages of the prior art overcome and create a process for the production of initial explosive in particular very small crystals (for example in the range from 0.5 to 30 μm, preferably from 1 to 20 .mu.m, particularly preferably from 1 to 10 .mu.m), wherein the crystal size obtained by setting process parameters largely controllable and where in each case a narrow and defined grain spectrum should be adjustable.
Gelöst wird die Aufgabe durch die Verwendung eines Mikrojetreaktors für die Herstellung von Initialsprengstoff, wobei die Ausgangslösungen zur Sprengstoffherstellung in dem Mikrojetreaktor durch jeweils eine Düse in einen von einem Reaktorgehäuse umschlossenen Reaktorraum auf einen gemeinsamen Kollisionspunkt gespritzt werden, über eine Öffnung in den Reaktorraum ein Gas eingeleitet wird und die entstehenden Initialsprengstoffkristalle zusammen mit der Flüssigkeit und überschüssigem Gas durch eine weitere Öffnung aus dem Reaktorgehäuse entfernt werden. Ein Mikrojetreaktor ist z.B. beschrieben in der WO 00/61275, wobei auf den gesamten Offenbarungsgehalt diese Druckschriftschrift hier ausdrücklich Bezug genommen wird.The problem is solved by the use of a microjet reactor for the Production of initial explosive, wherein the starting solutions for Explosives production in the microjet reactor through one nozzle at a time from a reactor housing enclosed reactor space on a Common collision point to be injected via an opening in the Reactor space, a gas is introduced and the resulting Initial explosive crystals along with the liquid and excess gas be removed through a further opening from the reactor housing. One Microjet reactor is e.g. described in WO 00/61275, wherein on the entire disclosure content of this document here express reference is taken.
Überraschend wurde gefunden, dass bei der Verwendung eines Mikrojetreaktors für die Herstellung von Initialsprengstoff dieser in einem engen, definierten und einstellbaren Kornspektrum gewonnen werden kann. Insbesondere ist es auf diese Weise möglich, einen Initialsprengstoff mit Kristallgrößen zwischen 0,5 bis 30 µm zu erhalten.Surprisingly, it has been found that when using a microjet reactor for the production of initial explosive this in a close, defined and adjustable grain spectrum can be obtained. In particular, it is up this way possible, an initial explosive with crystal sizes between 0.5 to To obtain 30 microns.
Die Größe der bei der Fällung entstehenden Sprengstoffkristalle lässt sich durch Variieren der Betriebsparameter reproduzierbar steuern. Dazu können der Durchmesser der reaktandenzuführenden Düsen, der Pumpendruck, die Temperaturen und Konzentrationen der Ausgangslösungen und die Menge des Hilfsgases variiert werden. Der Düsendurchmesser beträgt bevorzugt 10 bis 1000 µm, besonders bevorzugt 50 bis 500 µm und ganz besonders bevorzugt 50 bis 100 µm. Der Gesamtdurchfluss beträgt bevorzugt 10 bis 1000 ml/Minute, besonders bevorzugt 50 bis 500 ml/Minute. The size of the resulting explosive crystals in the precipitation can be through Varying the operating parameters reproducibly control. This can be the Diameter of the reactant supplying nozzles, the pump pressure, the Temperatures and concentrations of the starting solutions and the amount of Auxiliary gases are varied. The nozzle diameter is preferably 10 to 1000 microns, more preferably 50 to 500 microns and most preferably 50 to 100 μm. The total flow rate is preferably 10 to 1000 ml / minute, more preferably 50 to 500 ml / minute.
Durch die erfindungsgemäße Verwendung lassen sich bevorzugt folgende Initialsprengstoffe herstellen: Kaliumdinitrobenzofuroxanat, Bleiazid, Bleipikrat, Bleitrinitroresorcinat und Cäsiumdinitrobenzofuroxanat.The use according to the invention makes it possible to prefer the following Make initial explosives: potassium dinitrobenzofuroxanate, lead azide, lead picrate, Leadrinitic resorcinate and cesium dinitrobenzofuroxanate.
Ein weiterer Vorteil der erfindungsgemäßen Verwendung besteht darin, dass bedingt durch die definierte Kristallgröße des Initialsprengstoffes eine fraktionierte (und gefährliche) Siebung unterbleiben kann.Another advantage of the use according to the invention is that due to the defined crystal size of the initial explosive one fractionated (and dangerous) screening can be omitted.
Der Gegenstand der Erfindung wird anhand des folgenden Beispiels näher erläutert:The object of the invention will become more apparent from the following example explains:
In einem Mikrojetreaktor mit einem Reaktorraum von 2 mm Durchmesser und 50 mm Länge wurden über 2 Düsen mit einem Düsendurchmesser von 100 µm eine Natriumdibenzofuroxanatlösung mit einer Temperatur von 23 °C und mit einer Konzentration von 20 g/l und eine Kaliumnitratlösung mit einer Temperatur von 23 °C und mit einer Konzentration von 30 g/l bei einem jeweiligen Düsendruck von 100 bar zusammengegeben. Als Transportgas wurde Luft verwendet. Nach 2-minütiger Reaktion wurden ca. 1 l Reaktionsflüssigkeit mit einem Gehalt von ca. 5 g feinverteiltem Kaliumdinitrobenzofuroxanat erhalten.In a microjet reactor with a reactor space of 2 mm diameter and 50 mm length were via 2 nozzles with a nozzle diameter of 100 microns a Natriumdibenzofuroxanatlösung with a temperature of 23 ° C and with a Concentration of 20 g / l and a potassium nitrate solution with a temperature of 23 ° C and with a concentration of 30 g / l at a respective nozzle pressure of 100 bar combined. Air was used as transport gas. To 2 minutes of reaction were about 1 l of reaction liquid containing about 5 g of finely divided potassium dinitrobenzofuroxanate obtained.
Claims (6)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10334992 | 2003-07-31 | ||
| DE10334992A DE10334992A1 (en) | 2003-07-31 | 2003-07-31 | Use of a microjet reactor for the production of initial explosive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1505047A2 true EP1505047A2 (en) | 2005-02-09 |
| EP1505047A3 EP1505047A3 (en) | 2006-11-15 |
Family
ID=33547045
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP04017847A Withdrawn EP1505047A3 (en) | 2003-07-31 | 2004-07-28 | Use of a microjet reactor for manufacturing a primary explosive |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US20050188874A1 (en) |
| EP (1) | EP1505047A3 (en) |
| DE (1) | DE10334992A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011114089A1 (en) * | 2010-03-16 | 2011-09-22 | Qinetiq Limited | Mems detonator |
| CN108752150A (en) * | 2018-07-09 | 2018-11-06 | 山西壶化集团股份有限公司 | A kind of preparation method of KBKG detonating agents |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB741756A (en) * | 1953-02-24 | 1955-12-14 | Secr Defence Brit | Method for producing fine crystals of controlled particle size |
| FR2363536A1 (en) * | 1976-09-07 | 1978-03-31 | Imp Metal Ind Kynoch Ltd | Explosive esp. styphnate, for detonating ammunition, prodn. - in separate small quantities corresponding to specific requirements of weapon |
| US5156779A (en) * | 1989-04-27 | 1992-10-20 | E. I. Du Pont De Nemours And Company | Process and apparatus for producing ultrafine explosive particles |
| DE19501889A1 (en) * | 1994-01-24 | 1995-07-27 | Nof Corp | Prodn. of primer granulate useful in gas generator e.g. for car airbag |
| WO2000061275A2 (en) * | 1999-04-08 | 2000-10-19 | Bernd Penth | Method and device for carrying out chemical and physical processes |
| WO2001038264A1 (en) * | 1999-11-23 | 2001-05-31 | Technanogy, Llc | Composition and method for preparing oxidizer matrix containing dispersed metal particles |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2265230A (en) * | 1938-11-25 | 1941-12-09 | Western Cartridge Co | Basic lead styphnate and a process of making it |
| US2395860A (en) * | 1943-11-05 | 1946-03-05 | American Cyanamid Co | Preparation of crystalline materials |
| DE3926466C2 (en) * | 1989-08-10 | 1996-12-19 | Christoph Dipl Ing Caesar | Microreactor for carrying out chemical reactions of two chemical substances with strong heat |
| US20020119079A1 (en) * | 1999-12-10 | 2002-08-29 | Norbert Breuer | Chemical microreactor and microreactor made by process |
| DE10049200A1 (en) * | 2000-10-05 | 2002-04-11 | Clariant Gmbh | Process for the production of azo colorants |
-
2003
- 2003-07-31 DE DE10334992A patent/DE10334992A1/en not_active Withdrawn
-
2004
- 2004-07-28 EP EP04017847A patent/EP1505047A3/en not_active Withdrawn
- 2004-07-30 US US10/901,973 patent/US20050188874A1/en not_active Abandoned
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB741756A (en) * | 1953-02-24 | 1955-12-14 | Secr Defence Brit | Method for producing fine crystals of controlled particle size |
| FR2363536A1 (en) * | 1976-09-07 | 1978-03-31 | Imp Metal Ind Kynoch Ltd | Explosive esp. styphnate, for detonating ammunition, prodn. - in separate small quantities corresponding to specific requirements of weapon |
| US5156779A (en) * | 1989-04-27 | 1992-10-20 | E. I. Du Pont De Nemours And Company | Process and apparatus for producing ultrafine explosive particles |
| DE19501889A1 (en) * | 1994-01-24 | 1995-07-27 | Nof Corp | Prodn. of primer granulate useful in gas generator e.g. for car airbag |
| WO2000061275A2 (en) * | 1999-04-08 | 2000-10-19 | Bernd Penth | Method and device for carrying out chemical and physical processes |
| WO2001038264A1 (en) * | 1999-11-23 | 2001-05-31 | Technanogy, Llc | Composition and method for preparing oxidizer matrix containing dispersed metal particles |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011114089A1 (en) * | 2010-03-16 | 2011-09-22 | Qinetiq Limited | Mems detonator |
| GB2491225A (en) * | 2010-03-16 | 2012-11-28 | Qinetiq Ltd | Method of preparing explosives |
| GB2491225B (en) * | 2010-03-16 | 2013-05-01 | Qinetiq Ltd | MEMS detonator |
| EP2687811A1 (en) * | 2010-03-16 | 2014-01-22 | QinetiQ Limited | MEMS detonator |
| CN108752150A (en) * | 2018-07-09 | 2018-11-06 | 山西壶化集团股份有限公司 | A kind of preparation method of KBKG detonating agents |
Also Published As
| Publication number | Publication date |
|---|---|
| US20050188874A1 (en) | 2005-09-01 |
| EP1505047A3 (en) | 2006-11-15 |
| DE10334992A1 (en) | 2005-02-24 |
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