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EP1468739A1 - Agitator ball mill - Google Patents

Agitator ball mill Download PDF

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Publication number
EP1468739A1
EP1468739A1 EP04405182A EP04405182A EP1468739A1 EP 1468739 A1 EP1468739 A1 EP 1468739A1 EP 04405182 A EP04405182 A EP 04405182A EP 04405182 A EP04405182 A EP 04405182A EP 1468739 A1 EP1468739 A1 EP 1468739A1
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EP
European Patent Office
Prior art keywords
ball mill
grinding
agitator ball
good
mill according
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Granted
Application number
EP04405182A
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German (de)
French (fr)
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EP1468739B1 (en
Inventor
Martin Heinzelmann
Stefan Spornberger
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Willy A Bachofen AG
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Willy A Bachofen AG
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Application filed by Willy A Bachofen AG filed Critical Willy A Bachofen AG
Priority to PL04405182T priority Critical patent/PL1468739T3/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16—Mills in which a fixed container houses stirring means tumbling the charge
    • B02C17/163—Stirring means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16—Mills in which a fixed container houses stirring means tumbling the charge
    • B02C17/161—Arrangements for separating milling media and ground material

Definitions

  • the invention relates to a stirred ball mill with a Separator for separation of KleinstmahlMechn with a Diameter D ⁇ 0,1mm from the product.
  • Agitator ball mills for example, for crushing and dispersing solids in a liquid phase or used for the digestion of microorganisms.
  • agitator ball mills have a cylindrical, horizontal or vertical axis grinding chamber with various types Separators for separating the grinding media from Product in the product outlet area.
  • the housing of the grinding chamber of a stirred ball mill consists from one longitudinal wall and two at the two ends of the Longitudinal wall arranged end walls. It has a Feeding the ground good serving inlet and a for Discharge of the good serving good outlet.
  • In the Milling chamber is also a rotatable about the chamber axis Agitator arranged to be located in the mill To convey grinding media radially to the stirring shaft and thereby the continuously passed through the grinding chamber Good crushed by impact and shear forces or zu disperse.
  • a blockage of the outlet possibly caused Due to the tight tolerances at the good outlet, can be a striking Increase in pressure and the actual grinding and Prevent dispersing process.
  • grinding media will come out of the mill and the grinding agent Dispersion process increasingly deteriorates. moreover In this case, the millbase is contaminated with grinding media.
  • the invention is based on the object, a horizontal axis Agitator ball mill with a novel Separating member to create, not the aforementioned disadvantages and with which a good gently and evenly can be ground with KleinstmahlMechn, the one Have diameter D ⁇ 0.1 mm, without this the grinding chamber leave.
  • FIG. 1 shows a longitudinal section through a part of a horizontal grinding chamber with a separating element of the inventive type
  • FIG. 2 a shows a cross section through the separating element shown in FIG. 1
  • FIG. 2b shows a section along the line IIb of FIG. 2a
  • 3 shows a longitudinal section through a second embodiment of the invention
  • Figure 4 is a plan view of an alternative embodiment of a separating member of the inventive type.
  • the only partially shown in Figure 1 and as a whole designated 50 grinding chamber of a stirred ball mill has a housing 40 with a horizontal axis 60.
  • the Housing 40 has an elongated, substantially cylindrical Longitudinal wall 30 and two at both ends of the longitudinal wall 30 arranged end walls 35 and 36, of which the End wall 36 serving for feeding the ground material Good inlet 37 and the end wall 35 a for discharging the good serving outlet 38 has.
  • a stirrer 1 is arranged, the several, for example two, distributed along the axis 60, Paddle wheel-like impellers 2 has.
  • the axis 60th Coaxial shaft 4 of the agitator 1 is with her the end wall 36 piercing end to one in the drawing not shown drive device connected.
  • separating member 80 In the end wall 35 of the grinding chamber 50 is located a coaxial with the axis 60 arranged separating member 80, which with an external drive 18 is connected. This external Drive 18 displaces the separating member 80 in one of the agitator. 1 independent rotary motion.
  • the regrind outlet 38 leads coaxial with the axis 60 from the separator 80 for rotary feedthrough 17th
  • a seal 45 is provided in the end wall 35, which ensures that no regrind with grinding media the annular gap between separating device 80 and End wall 35 penetrates through to the outside. This seal 45 complies with the requirements for grinding media size ⁇ 0.1mm.
  • the two disks 5 arranged parallel to one another and 7 of the separating member 80 are at a predetermined distance from each other. This is done by several, around the disk center symmetrically distributed, from the disk edge inwards leading, in plan view arcuate conveyor or Wing elements 12 determined.
  • the circular disc 7 sits on the wing elements 12 and is about this with the disc. 5 detachably or permanently connected.
  • a circular cavity 8 between the discs. 5 and Figure 7 may further include a ring cage 10 with one at its end Be located outer surface mesh screen ring 6 inserted.
  • the Ring cage 10 is preferably with O-rings 11th pressed and sealed and can be either with or without Screen plate ring 6 to be mounted. The choice of the use of the Siebblechringes 6 can on the respective Product properties are adjusted.
  • This can be for example primarily products from nanotechnology, but also um Dye suspension, enamel paints, printing inks, Agrochemicals, filler suspension, video tape Coating, cosmetics, food, pharmaceutical or Act microorganisms.
  • the use of Smaller grinding media D ⁇ 0.1 mm is mainly used to Break up agglomerates and aggregates without the Primary particles are destroyed.
  • rotating separator 80 is now formed and measure that from the grinding media and the ground and / or dispersed Good formed mixture in the interspace between the two disks 5 and 7 flows, whereupon due to the centrifugal force and the different specific Density the grinding media serving for grinding the conveying elements 12 separated from the material to be ground and back into the Interior 3 of the grinding chamber 50 are conveyed.
  • the regrind itself passes through the circular cavity 8 of the Separator 80 through the Gutauslauf 38 where it Grinding chamber 50 leaves. By the rotation of the separating member 80th the product must pass through this separator overcome relative to the centrifugal force a relative pressure.
  • the peripheral speed of the separating member 80th and the radial flow velocity in the Flow channels are the determining Operating variables, the peripheral speed of the separating member 80th and the radial flow velocity in the Flow channels.
  • the peripheral speed is determined by the Speed determined.
  • the radial flow velocity results from the free cross section and the volume flow of the product through the pump.
  • the grinding chamber 51 shown in FIG. 3 corresponds essentially the grinding chamber according to FIG. 1. That is,
  • the separating element designated here by 82 is located opposite the agitator 22 on a separate drive shaft and it carries the regrind outlet 39 coaxial with the axis 61 of Separator 82 for rotary feedthrough 17.
  • the drive 28 is in arranged in this case parallel to the axis 61 and offset the the separating member 83 bearing shaft via a sub / translation in a direction independent of the agitator 22 rotational movement.
  • a sieve scraper 65 which serves, if necessary, stuck on the sieve 6 Strip off grinding media, so that no adverse Pressure increase takes place and all grinding media through the Rotational movement of the separating member 82 of the grinding chamber returned can be.
  • FIG. 4 in the form of a paddle wheel-like Separator 85 differs from the above described separating members 80 and 82 in that between the arcuate wing elements 12 additionally straight or slightly curved conveying elements 86 are provided, the extend inwards from the edge of the disc. This forms inside a secondary flow.
  • the separating members 80 and 82 optionally provided with or without straight conveying elements 86 be the conveying elements 12 and 86 either to the Slices 5 or 7 may be attached and it may be the parting organs optionally equipped with or without screen plate ring 6 his.
  • stirring elements described above numerically arbitrary with each other and / or with others Known stirrers are combined and it can the grinding chamber additionally with pressure relief valves or the like be designed to withstand any pressure fluctuations, especially to compensate for pressure increases.
  • longitudinal wall of the grinding chamber in addition of a cylindrical Sheath be wrapped, which together with her in the Cross-section circular, space bounded in the to Cooling or heating of the existing in the interior of a good Cooling or heating fluid can be introduced.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Crushing And Grinding (AREA)
  • Powder Metallurgy (AREA)

Abstract

The agitating ball mill has separating system formed from a separating component (80) which has two circular discs (5,7) co-axial to the chamber axis, and between which are installed several transporting or vane elements distributed symmetrically around the disc center point and leading inwards from the disc edge. During the operation of the separating device the transporting or vane elements create a back pressure on the material and milling body mix so by centrifugal force and different specific densities the milling bodies are separated from the product and transported back to the inner chamber (3) of the mill.

Description

Die Erfindung betrifft eine Rührwerkskugelmühle mit einem Trennorgan zur Trennung von Kleinstmahlkörpern mit einem Durchmesser D ≤ 0,1mm vom Produkt.The invention relates to a stirred ball mill with a Separator for separation of Kleinstmahlkörpern with a Diameter D ≤ 0,1mm from the product.

Rührwerkskugelmühlen werden beispielsweise zur Zerkleinerung und Dispergierung von Feststoffen in einer Flüssigkeitsphase oder zum Aufschluss von Mikroorganismen verwendet.Agitator ball mills, for example, for crushing and dispersing solids in a liquid phase or used for the digestion of microorganisms.

Auf dem Markt bekannte und für den kontinuierlichen Betrieb vorgesehene Rührwerkskugelmühlen besitzen eine zylindrische, horizontal- oder vertikalachsige Mahlkammer mit verschiedenartigen Trennorganen zum Abtrennen der Mahlkörper vom Produkt im Produktauslassbereich.Known in the market and for continuous operation provided agitator ball mills have a cylindrical, horizontal or vertical axis grinding chamber with various types Separators for separating the grinding media from Product in the product outlet area.

Das Gehäuse der Mahlkammer einer Rührwerkskugelmühle besteht aus einer Längswand und zwei an den beiden Enden der Längswand angeordneten Abschlusswänden. Es weist einen zum Zuführen des Mahlgutes dienenden Gut-Einlass und einen zum Abführen des Gutes dienenden Gut-Auslass auf. In der Mahlkammer ist zudem ein um die Kammerachse drehbares Rührwerk angeordnet, um die in der Mühle befindlichen Mahlkörper radial zur Rührwelle zu befördern und dadurch das kontinuierlich durch die Mahlkammer hindurchgeleitete Gut durch Stoss- und Scherkräfte zu zerkleinern bzw. zu dispergieren.The housing of the grinding chamber of a stirred ball mill consists from one longitudinal wall and two at the two ends of the Longitudinal wall arranged end walls. It has a Feeding the ground good serving inlet and a for Discharge of the good serving good outlet. In the Milling chamber is also a rotatable about the chamber axis Agitator arranged to be located in the mill To convey grinding media radially to the stirring shaft and thereby the continuously passed through the grinding chamber Good crushed by impact and shear forces or zu disperse.

Bei der kontinuierlichen Durchströmung einer Rührwerkskugelmühle tritt abhängig von der Strömungsgeschwindigkeit und von der Viskosität der Mahlgutsuspension eine Schleppkraft auf, die auf die Mahlkörper wirkt. Dadurch werden die Mahlkörper mit dem Mahlgut vom Eintritt in die Mahlzone bis zum Trennorgan im Bereich des Gut-Auslasses mitgeschleppt. Dies kann zu einer Verpressung der Mahlkörper vor dem Trennorgan führen, welche mit erhöhtem Verschleiss und erhöhter Verstopfungsgefahr verbunden ist. Bei Kleinstmahlkörpern mit einem Durchmesser D ≤ 0,1mm nimmt die Mitschleppwirkung des Produktes um ein Vielfaches zu und ist bei Feinstmahlungen und -dispergierungen insbesondere bei hohen Durchsatzraten kritisch.In the continuous flow through an agitator ball mill occurs depending on the flow velocity and the viscosity of the meal stock suspension has a drag force on, which acts on the grinding media. This will be the Mahlkörper with the material to be ground from the entrance to the grinding zone until entrained to the separating element in the region of the good outlet. This can lead to a compression of the grinding media before Separating lead, which with increased wear and increased risk of clogging is connected. at Kleinstmahlkörpern with a diameter D ≤ 0,1mm takes the Entrainment of the product many times and is in Feinstmahlungen and -dispergierungen in particular at high throughput rates critical.

Es sind Rührwerkskugelmühlen bekannt, die zur Lösung dieses Problems verschiedenste Konstruktionen aufweisen, in der Weise, dass den mitgeschleppten Mahlkörpern eine Zirkulation in der Mühle mit Rückführung in die Mahlzone ermöglicht wird. Die bekannten Lösungen sind aber für Mahlkörper D ≤ 0,1mm sehr oft ungenügend.Agitator ball mills are known which are used to solve this problem Problems have a variety of constructions, in the Way that the entrained Mahlkörpern a circulation in the mill with return to the grinding zone is made possible. However, the known solutions are for grinding media D ≤ 0,1mm very often insufficient.

Bei weiteren bekannten Abtrennsystemen, wie zum Beispiel bei der Verwendung von sogenannten Spaltsiebpatronen, gestaltet sich die Fertigung mit kleinen Spaltweiten von ≤ 0,05mm als sehr schwierig, die zudem in der Praxis kaum brauchbar sind. Zudem ist in diesen Fällen die Wahrscheinlichkeit, dass das Sieb verstopft wird, sehr hoch, falls Mahlkörper mit D ≤ 0,1mm benützt werden müssen, was in der Nanotechnologie und somit auch in der Herstellung von Nanoteilchen nötig ist.In other known separation systems, such as in the use of so-called slotted screen cartridges designed the production with small gap widths of ≤ 0.05mm as very difficult, which also hardly usable in practice are. In addition, in these cases, the probability that the sieve is clogged, very high, if grinding media with D ≤ 0.1mm, which is used in nanotechnology and thus also in the production of nanoparticles is necessary.

Ein weiteres Problem entsteht durch den hohen Druckverlust aufgrund der Anreicherung von Mahlkörpern auf dem Sieb. Bei der sogenannten Reibspaltausführung ist eine ausserordentlich hohe Präzision in der Herstellung erforderlich, um die kleinen Reibspalte von ≤ 0.05mm im ganzen Produktionsverlauf zu gewährleisten.Another problem arises from the high Pressure loss due to the accumulation of grinding media on the sieve. In the so-called Reibspaltausführung is a exceptionally high manufacturing precision required to have the small friction gaps of ≤ 0.05mm in throughout the production process.

Aus der Offenlegungschrift DE 44 12 408 A1 ist es bekannt, in einer horizontalen Mühle die Mahlkörper zwar durch eine Vorklassierscheibe und einem rotierenden Käfig vom Auslasskörper zum Teil fernzuhalten, dennoch können durch die achsnahen Bohrungen in der Trenneinrichtung, durch die das Produkt hindurchströmen muss, Mahlkörper mitgeschleppt werden und somit zum Auslasskörper gelangen. Da die Mitschleppwirkung des Mahlgutes mit der Abnahme des Mahlkörperdurchmessers um ein Vielfaches zunimmt, ist für solche Anwendungen die Verwendung einer entsprechenden Abtrennvorrichtung, die die Mahlkörper wirksam und zuverlässig vom Produktgut trennt, somit unumgänglich.It is from the disclosure document DE 44 12 408 A1 known, in a horizontal mill, the grinding media though through a Vorlassierscheibe and a rotating cage from Partially keep outlet body, but still can by the Near-axis holes in the separator through which the Product must flow through, Mahlkörper be entrained and thus reach the outlet body. Because the Entrainment effect of the ground material with the decrease of the Mahlkörperdurchmessers increases by a multiple, is for Such applications require the use of an appropriate Separator, which makes the grinding media effective and Reliably separates from the product, thus inevitable.

Eine Verstopfung des Auslasses, eventuell hervorgerufen durch die engen Toleranzen am Gut-Auslass, kann zu einem markanten Druckanstieg führen und den eigentlichen Mahl- und Dispergierprozess unterbinden. Bei Versagen der Abtrennfunktion treten zudem Mahlkörper aus der Mühle aus und der Mahlund Dispergierprozess verschlechtert sich zunehmend. Zudem wird in diesem Fall das Mahlgut mit Mahlkörpern verunreinigt.A blockage of the outlet, possibly caused Due to the tight tolerances at the good outlet, can be a striking Increase in pressure and the actual grinding and Prevent dispersing process. In case of failure of the separation function In addition, grinding media will come out of the mill and the grinding agent Dispersion process increasingly deteriorates. moreover In this case, the millbase is contaminated with grinding media.

Weitere Vorschläge zur Vermeidung des Verstopfens der Trenneinrichtung werden hauptsächlich für vertikale Rührwerkskugelmühlen beschrieben. Eine solche Erfindung wird in Patent EP 0 771 591 A1 gezeigt. Dabei handelt es sich um eine vertikale Rührwerkskugelmühle, in welcher das Mahlgut einen von Mahlkörpern beschickten Mahlbehälter und einen auf dem Rührorgan vor dem Auslauf sitzenden Separator von unten nach oben durchströmt. Da der Separator kein Sieb, Filter oder anderes Mahlkörperrückhaltesystem besitzt, lässt sich diese Erfindung nicht bei einer horizontalachsigen Mühle verwenden, da beim Befüllen mit Mahlkörper bzw. beim Entleeren des Mahlgutes nach Beendigung des Mahlvorganges mit Mahlkörperaustritt beim Auslass zu rechnen ist, welcher das Mahlgut mit Mahlkörper verunreinigt. Ebenfalls ist die Zentrifugalbeschleunigung der Mahlkörper von der Geschwindigkeit der Rührscheiben abhängig und somit auch von der Eigenschaft des Produktes, was zum Beispiel bei scherempfindlichen Produkten und somit tiefen Drehzahlen zu einer zu geringen Zentrifugalbeschleunigung der Mahlkörper führen kann bzw. zum Austritt der Mahlkörper. Vertikale Rührwerkskugelmühlen weisen auch den Nachteil der inhomogenen Mahlkörperverteilung in der Mahlkammer auf, was zu einer schlechten Mahl- bzw. Diespergierleistung führt.Other proposals to avoid clogging the Separator are mainly used for vertical Agitator ball mills described. Such an invention will in patent EP 0 771 591 A1. It refers to a vertical agitator ball mill, in which the ground material one of Mahlkörpern loaded grinding container and a the stirrer sitting in front of the outlet separator from below flows through the top. Since the separator no sieve, filter or other Mahlkörperrückhaltesystem, can be this invention not in a horizontal axis mill use, as when filling with grinding media or when Emptying the ground material after completion of the grinding process with Mahlkörperaustritt is expected at the outlet, which is the Ground material contaminated with grinding media. Also is the Centrifugal acceleration of the grinding media of the Speed of the stirring discs dependent and therefore also of the property of the product, what for example shear sensitive products and thus low speeds too low a centrifugal acceleration of the grinding media can lead or to the exit of the grinding media. vertical Agitator ball mills also have the disadvantage of inhomogeneous Mahlkörperverteilung in the grinding chamber on, resulting in a poor grinding or dispersing performance results.

Der Erfindung liegt nun die Aufgabe zugrunde, eine horizontalachsige Rührwerkskugelmühle mit einem neuartigen Trennorgan zu schaffen, das die vorgenannten Nachteile nicht aufweist und mit welcher ein Gut schonend und gleichmässig mit Kleinstmahlkörpern gemahlen werden kann, die einen Durchmesser D ≤ 0,1 mm besitzen, ohne dass diese den Mahlraum verlassen.The invention is based on the object, a horizontal axis Agitator ball mill with a novel Separating member to create, not the aforementioned disadvantages and with which a good gently and evenly can be ground with Kleinstmahlkörpern, the one Have diameter D ≤ 0.1 mm, without this the grinding chamber leave.

Diese Aufgabe wird durch eine Rührwerkskugelmühle mit den Merkmalen des Anspruchs 1 gelöst.This object is achieved by an agitator ball mill with the Characteristics of claim 1 solved.

Vorteilhafte Ausführungsformen der Erfindung sind Gegenstand der abhängigen Ansprüche.Advantageous embodiments of the invention are the subject the dependent claims.

Nachfolgend werden anhand der Zeichnung Ausführungsbeispiele der Erfindung beschrieben. In der Zeichnung zeigt
   die Figur 1 einen Längsschnitt durch einen Teil einer horizontalen Mahlkammer mit einem Trennorgan der erfindungsgemässen Art,
   die Figur 2a eine Querschnitt durch das in der Figur 1 dargestellte Trennorgan,
   die Figur 2b einen Schnitt entlang der Linie IIb der Figur 2a,
   die Figur 3 einen Längsschnitt durch eine zweite Ausführungsform der Erfindung,
   die Figur 4 eine Draufsicht auf eine alternative Ausführung eines Trennorgans der erfindungsgemässen Art.Hereinafter, embodiments of the invention will be described with reference to the drawings. In the drawing shows
1 shows a longitudinal section through a part of a horizontal grinding chamber with a separating element of the inventive type,
FIG. 2 a shows a cross section through the separating element shown in FIG. 1,
FIG. 2b shows a section along the line IIb of FIG. 2a,
3 shows a longitudinal section through a second embodiment of the invention,
Figure 4 is a plan view of an alternative embodiment of a separating member of the inventive type.

Die in der Figur 1 nur zum Teil dargestellte und als ganzes mit 50 bezeichnete Mahlkammer einer Rührwerkskugelmühle weist ein Gehäuse 40 mit einer horizontalen Achse 60 auf. Das Gehäuse 40 besitzt dabei eine längliche, im Wesentlichen zylindrische Längswand 30 sowie zwei an beiden Enden der Längswand 30 angeordnete Abschlusswände 35 und 36, von denen die Abschlusswand 36 einen zum Zuführen des Mahlgutes dienenden Gut-Einlass 37 und die Abschlusswand 35 einen zum Abführen des Gutes dienenden Gut-Auslass 38 aufweist.The only partially shown in Figure 1 and as a whole designated 50 grinding chamber of a stirred ball mill has a housing 40 with a horizontal axis 60. The Housing 40 has an elongated, substantially cylindrical Longitudinal wall 30 and two at both ends of the longitudinal wall 30 arranged end walls 35 and 36, of which the End wall 36 serving for feeding the ground material Good inlet 37 and the end wall 35 a for discharging the good serving outlet 38 has.

Im Innenraum 3 ist ein Rührwerk 1 angeordnet, das mehrere, beispielsweise zwei, entlang der Achse 60 verteilte, Schaufelrad-artige Rührorgane 2 aufweist. Die zur Achse 60 koaxiale Welle 4 des Rührwerks 1 ist dabei mit ihrem die Abschlusswand 36 durchstossenden Ende an einer in der Zeichnung nicht dargestellten Antriebsvorrichtung angeschlossen.In the interior 3, a stirrer 1 is arranged, the several, for example two, distributed along the axis 60, Paddle wheel-like impellers 2 has. The axis 60th Coaxial shaft 4 of the agitator 1 is with her the end wall 36 piercing end to one in the drawing not shown drive device connected.

In der Abschlusswand 35 der Mahlkammer 50 befindet sich ein koaxial zur Achse 60 angeordnetes Trennorgan 80, das mit einem externen Antrieb 18 verbunden ist. Dieser externe Antrieb 18 versetzt das Trennorgan 80 in eine vom Rührwerk 1 unabhängige Drehbewegung. Der Mahlgut-Auslass 38 führt koaxial zur Achse 60 vom Trennorgan 80 zur Drehdurchführung 17.In the end wall 35 of the grinding chamber 50 is located a coaxial with the axis 60 arranged separating member 80, which with an external drive 18 is connected. This external Drive 18 displaces the separating member 80 in one of the agitator. 1 independent rotary motion. The regrind outlet 38 leads coaxial with the axis 60 from the separator 80 for rotary feedthrough 17th

In der Abschlusswand 35 ist eine Dichtung 45 vorgesehen, die gewährleistet, dass kein Mahlgut mitsamt Mahlkörpern aus dem Ringspalt zwischen Abtrennvorrichtung 80 und Abschlusswand 35 hindurch nach aussen dringt. Diese Dichtung 45 entspricht den Anforderungen an die Mahlkörpergrösse ≤ 0.1mm.In the end wall 35, a seal 45 is provided, which ensures that no regrind with grinding media the annular gap between separating device 80 and End wall 35 penetrates through to the outside. This seal 45 complies with the requirements for grinding media size ≤ 0.1mm.

Wie aus den Figuren 1, 2a und 2b ersichtlich ist, besitzt das Trennorgan 80 eine auf der Welle 9 sitzende und auf dieser lösbar befestigte Kreisscheibe 5 und eine der Abschlusswand 35 zugewandte Kreisscheibe 7 mit einem koaxial zur Achse 60 angeordneten, rohrartigen Gut-Auslauf 38, der in die Abschlusswand 35 hineinragt und in der Drehdurchführung 17 endet.As can be seen from FIGS. 1, 2a and 2b the separating member 80 a sitting on the shaft 9 and on this releasably secured circular disc 5 and one of the end wall 35 facing circular disc 7 with a coaxial to the axis 60 arranged, tubular Good outlet 38, in the end wall 35 protrudes and in the rotary feedthrough 17th ends.

Die beiden parallel zueinander angeordneten Scheiben 5 und 7 des Trennorgans 80 stehen in vorbestimmtem Abstand voneinander. Dieser wird durch mehrere, um den Scheibenmittelpunkt symmetrisch verteilte, vom Scheibenrand nach innen führende, in der Draufsicht bogenförmige Förder- bzw. Flügelelemente 12 bestimmt. Im bevorzugten Ausführungsbeispiel gemäss den Figuren 2a, 2b sitzt die Kreisscheibe 7 auf den Flügelelementen 12 und ist über diese mit der Scheibe 5 lösbar oder unlösbar verbunden.The two disks 5 arranged parallel to one another and 7 of the separating member 80 are at a predetermined distance from each other. This is done by several, around the disk center symmetrically distributed, from the disk edge inwards leading, in plan view arcuate conveyor or Wing elements 12 determined. In the preferred embodiment According to the figures 2a, 2b, the circular disc 7 sits on the wing elements 12 and is about this with the disc. 5 detachably or permanently connected.

In einen kreisförmigen Hohlraum 8 zwischen den Scheiben 5 und 7 kann ferner ein Ringkäfig 10 mit einem an seiner Aussenfläche befindlichen Siebblechring 6 eingelegt sein. Der Ringkäfig 10 wird dabei vorzugsweise mit O-Ringen 11 verpresst und abgedichtet und kann wahlweise mit oder ohne Siebblechring 6 montiert sein. Die Wahl des Einsatzes des Siebblechringes 6 kann auf die jeweiligen Produkteigenschaften angepasst werden.In a circular cavity 8 between the discs. 5 and Figure 7 may further include a ring cage 10 with one at its end Be located outer surface mesh screen ring 6 inserted. Of the Ring cage 10 is preferably with O-rings 11th pressed and sealed and can be either with or without Screen plate ring 6 to be mounted. The choice of the use of the Siebblechringes 6 can on the respective Product properties are adjusted.

Beim Betrieb einer die Mahlkammer 50 aufweisenden Rührwerkskugelmühle wird durch den Einlass 37 und in Pfeilrichtung 71 ein zu mahlendes oder in einer Flüssigkeit zu dispergierendes Gut in flüssiger Form kontinuierlich in den Innenraum 3 der Mahlkammer 50 geführt und in diesem zum Mahlgut-Auslass 38 hinbefördert. Hierbei kann es sich beispielsweise vornehmlich um Produkte aus der Nanotechnologie, aber auch um Farbstoffsuspension, Lackfarben, Druckfarben, Agrochemikalien, Füllstoffsuspension, Video-Tape Beschichtungsmasse, Kosmetika, Nahrungsmittel, Pharma oder Mikroorganismen handeln. Die im Innenraum 3 der Mahlkammer 50 vorhandenen Mahlkörper vermahlen und/oder dispergieren während des Betriebes der Rührwerkskugelmühle das kontinuierlich durch die Mahlkammer 50 hindurchgeleitete Gut, worauf das in der Mahlkammer erzeugte Produkt diese - in einem kontinuierlichen Flüssigkeitsstrom - durch das Trennorgan 80 in Pfeilrichtung 72 verlässt. Der Einsatz von Kleinst-Mahlkörper D ≤ 0,1 mm dient hauptsächlich dazu, die Agglomerate und Aggregate aufzubrechen ohne dass dadurch die Primärteilchen zerstört werden.During operation of the grinding chamber 50 having agitator ball mill is through the inlet 37 and in the direction of the arrow 71 to be pulverized or dispersed in a liquid Good in liquid form continuously in the interior 3 of the grinding chamber 50 out and in this to the grinding stock outlet 38 transported. This can be for example primarily products from nanotechnology, but also um Dye suspension, enamel paints, printing inks, Agrochemicals, filler suspension, video tape Coating, cosmetics, food, pharmaceutical or Act microorganisms. The in the interior 3 of the grinding chamber 50th grind and / or disperse existing grinding media during operation of the agitator ball mill that continuously Good passed through the grinding chamber 50, whereupon the product produced in the grinding chamber this - in a continuous stream of liquid - through the Separator 80 leaves in the direction of arrow 72. The use of Smaller grinding media D ≤ 0.1 mm is mainly used to Break up agglomerates and aggregates without the Primary particles are destroyed.

Das durch den Antrieb 18 angetriebene in Pfeilrichtung 81 (Fig. 2a) rotierende Trennorgan 80 ist nun derart ausgebildet und bemessen, dass das aus den Mahlkörpern und dem gemahlenen und/oder dispergierten Gut gebildete Gemisch in den Zwischenraum zwischen den beiden Scheiben 5 und 7 einströmt, worauf aufgrund der Zentrifugalkraft und der unterschiedlichen spezifischen Dichte die zum Mahlen dienenden Mahlkörper durch die Förderelemente 12 vom Mahlgut getrennt und zurück in den Innenraum 3 der Mahlkammer 50 befördert werden. Das Mahlgut selbst gelangt durch den kreisförmigen Hohlraum 8 des Trennorgans 80 hindurch zum Gutauslauf 38, wo es die Mahlkammer 50 verlässt. Durch die Rotation des Trennorgans 80 muss das Produkt beim Durchströmen dieses Trennorgans entgegen der Fliehkraft einen relativen Druck überwinden. Dieser Druck, der je nach Betriebszustand zwischen 0.5 und 3bar liegt, wird durch die nicht dargestellte Speisepumpe aufgebracht. Dieser Belastung entsprechend muss das Gehäuse des Trennorgans 80 und ebenso die Dichtung 45 auf der Antriebswelle 9 druckfest ausgeführt sein, für letztere ist dabei in den meisten Fällen die Verwendung einer doppelten Gleitringdichtung erforderlich.The driven by the drive 18 in the direction of arrow 81 (Fig. 2a) rotating separator 80 is now formed and measure that from the grinding media and the ground and / or dispersed Good formed mixture in the interspace between the two disks 5 and 7 flows, whereupon due to the centrifugal force and the different specific Density the grinding media serving for grinding the conveying elements 12 separated from the material to be ground and back into the Interior 3 of the grinding chamber 50 are conveyed. The regrind itself passes through the circular cavity 8 of the Separator 80 through the Gutauslauf 38 where it Grinding chamber 50 leaves. By the rotation of the separating member 80th the product must pass through this separator overcome relative to the centrifugal force a relative pressure. This pressure, depending on the operating condition between 0.5 and 3bar, is by the feed pump, not shown applied. According to this load, the housing must the separating member 80 and also the seal 45 on the Drive shaft 9 to be executed pressure-resistant, for the latter is doing so in most cases the use of a double Mechanical seal required.

Um Mahlkörper zu trennen sind die bestimmenden Betriebsgrössen die Umfangsgeschwindigkeit des Trennorgans 80 und die radiale Strömungsgeschwindigkeit in den Strömungskanälen. Die Umfangsgeschwindigkeit wird durch die Drehzahl bestimmt. Die radiale Strömungsgeschwindigkeit ergibt sich aus dem freien Querschnitt und dem Volumenstrom des Produktes durch die Pumpe.To separate grinding media are the determining Operating variables, the peripheral speed of the separating member 80th and the radial flow velocity in the Flow channels. The peripheral speed is determined by the Speed determined. The radial flow velocity results from the free cross section and the volume flow of the product through the pump.

Die in der Figur 3 dargestellte Mahlkammer 51 entspricht im wesentlichen der Mahlkammer gemäss Figur 1. Das heisst, das hier mit 82 bezeichnete Trennorgan befindet sich gegenüber dem Rührwerk 22 auf einer separaten Antriebswelle und es führt der Mahlgut-Auslass 39 koaxial zur Achse 61 vom Trennorgan 82 zur Drehdurchführung 17. Der Antrieb 28 ist in diesem Fall parallel zur Achse 61 angeordnet und versetzt die das Trennorgan 83 tragende Welle über eine Unter/Übersetzung in eine vom Rührwerk 22 unabhängige Drehbewegung. Zusätzlich ist in dieser Variante noch ein Siebabstreifer 65 vorgesehen, der dazu dient, allenfalls auf dem Sieb 6 festsitzende Mahlkörper abzustreifen, so dass keine nachteilige Druckerhöhung stattfindet und alle Mahlkörper durch die Drehbewegung des Trennorgans 82 der Mahlkammer zurückgeführt werden können.The grinding chamber 51 shown in FIG. 3 corresponds essentially the grinding chamber according to FIG. 1. That is, The separating element designated here by 82 is located opposite the agitator 22 on a separate drive shaft and it carries the regrind outlet 39 coaxial with the axis 61 of Separator 82 for rotary feedthrough 17. The drive 28 is in arranged in this case parallel to the axis 61 and offset the the separating member 83 bearing shaft via a sub / translation in a direction independent of the agitator 22 rotational movement. additionally If a sieve scraper 65 is provided in this variant, which serves, if necessary, stuck on the sieve 6 Strip off grinding media, so that no adverse Pressure increase takes place and all grinding media through the Rotational movement of the separating member 82 of the grinding chamber returned can be.

Das in der Figur 4 in Ansicht dargestellte Schaufelrad-artige Trennorgan 85 unterscheidet sich von den vorstehend beschriebenen Trennorganen 80 und 82 dadurch, dass zwischen den bogenförmigen Flügelelementen 12 noch zusätzlich gerade oder leicht gekrümmte Förderelemente 86 vorgesehen sind, die sich vom Scheibenrand nach innen erstrecken. Dadurch bildet sich im Innern eine sekundäre Strömung. The illustrated in Figure 4 in the form of a paddle wheel-like Separator 85 differs from the above described separating members 80 and 82 in that between the arcuate wing elements 12 additionally straight or slightly curved conveying elements 86 are provided, the extend inwards from the edge of the disc. This forms inside a secondary flow.

An dieser Stelle sei noch darauf hingewiesen, dass bei einer zur Drehrichtung der Rührwerkswelle entgegengesetzten Rotation des Trennorgans, die Förderelemente gegenüber den in den Figuren 2 und 4 gezeichneten Elementen 12 bzw. 86 selbstverständlich spiegelverkehrt ausgebildet bzw. angeordnet sind.At this point it should be noted that at one opposite to the direction of rotation of the agitator shaft Rotation of the separating element, the conveying elements opposite to in Figures 2 and 4 drawn elements 12 and 86, of course mirrored trained or arranged are.

Das erfindungsgemässe Abtrennsystem einer Rührwerkskugelmühle für Kleinst-Mahlkörper mit einem Durchmesser D ≤ 0,1 mm weist gegenüber den bekannten Abtrennsystemen folgende Vorteile auf:

  • Die Rückhaltung der Kleinst-Mahlkörper im Mahlraum ist durch die geregelte und von der Rührwellen-Drehzahl unabhängige Einstellung der Drehzahl es Trennorgans gewährleistet.
  • Die Herstellungsproblematik der Bauteile ist entschärft worden.
  • Die Verstopfungsproblematik am Spaltsieb und Siebblech ist durch die Verwendung von einfachen dünnen Geweben entschärft oder beim Weglassen der Siebe eliminiert worden.
  • Die Belastung der Abtrennteile ist unbedeutend.
  • Verschleiss am Reibspalt ist nicht existent.
  • Die Herstellungsprobleme einer sehr engen und genauen Reibspaltkonstruktion sind eliminiert.
The separation system according to the invention of an agitator ball mill for very small grinding media with a diameter D ≦ 0.1 mm has the following advantages over the known separation systems:
  • The retention of the smallest grinding media in the grinding chamber is ensured by the regulated and independent of the stirring shaft speed setting the speed of the separating member.
  • The manufacturing problem of the components has been defused.
  • The clogging problem on the slotted screen and screen plate has been defused by the use of simple thin fabrics or eliminated in the omission of the screens.
  • The burden of the separation parts is insignificant.
  • Wear on the friction gap is nonexistent.
  • The manufacturing problems of a very tight and accurate friction gap design are eliminated.

Es sei an dieser Stelle darauf hingewiesen, dass die anhand der Figuren 1 bis 3 beschriebenen Mahlkammern, Rühr- und Trennorgane nur eine Auswahl von mehreren möglichen Ausführungsformen der Erfindung darstellen und in verschiedener Hinsicht geändert werden können.It should be noted at this point that the basis 1 to 3 described grinding chambers, stirring and Separators only a selection of several possible embodiments represent the invention and in various Respects can be changed.

So können beispielsweise die Trennorgane 80 und 82 wahlweise mit oder ohne geraden Förderelementen 86 versehen werden, die Förderelemente 12 und 86 entweder sowohl an den Scheiben 5 oder 7 befestigt sein und es können die Trennorgane wahlweise mit oder ohne Siebblechring 6 ausgestattet sein. Auch sind die Baugrössen der Trennorgane von den zu wählenden Umfangsgeschwindigkeiten abhängig und können von Fall zu Fall stark variieren.For example, the separating members 80 and 82 optionally provided with or without straight conveying elements 86 be the conveying elements 12 and 86 either to the Slices 5 or 7 may be attached and it may be the parting organs optionally equipped with or without screen plate ring 6 his. Also, the sizes of the separating elements of the zu depending on peripheral speeds and can of Vary greatly from case to case.

Ferner können die vorstehend beschriebenen Rührorganen zahlenmässig beliebig miteinander und/oder auch mit anderen bekannten Rührorganen kombiniert werden und es kann die Mahlkammer noch zusätzlich mit Druckentlastungsventilen oder dergleichen ausgebildet sein, um allfällige Druckschwankungen, insbesondere Druckerhöhungen auszugleichen. Schliesslich kann die Längswand der Mahlkammer noch zusätzlich von einem zylindrischen Mantel umhüllt sein, der mit ihr zusammen einen im Querschnitt kreisförmigen, Zwischenraum begrenzt, in den zum Kühlen oder Erwärmen des im Innenraum vorhandenen Gutes ein Kühl- oder Heizfluid eingeleitet werden kann.Furthermore, the stirring elements described above numerically arbitrary with each other and / or with others Known stirrers are combined and it can the grinding chamber additionally with pressure relief valves or the like be designed to withstand any pressure fluctuations, especially to compensate for pressure increases. Finally, can the longitudinal wall of the grinding chamber in addition of a cylindrical Sheath be wrapped, which together with her in the Cross-section circular, space bounded in the to Cooling or heating of the existing in the interior of a good Cooling or heating fluid can be introduced.

Claims (7)

Zum Fein- und Feinstmahlen eines Gutes dienende, kontinuierlich arbeitende horizontale Rührwerkskugelmühle mit einer zylindrischen oder konischen, zur Aufnahme von Mahlkörpern dienenden Mahlkammer (50, 51) einem am Ende der Mahlkammer (50, 51) angeordneten und in den Innenraum (3) der Mahlkammer (50, 51) mündenden Gut-Einlass (37), einem am anderen Ende der Mahlkammer angeordneten und aus dem Innenraum (3) herausführenden Gut-Auslass (38, 39) sowie einem mehrere Rührorgane (2) aufweisenden und zur Kammerachse (60) koaxialen Rührwerk (1, 22) und einem vor dem Gut-Auslass (38, 39) angeordneten separat angetriebenes Abtrennsystem, das die Mahlkörper vom gemahlenen Gut trennt und zurück in den Innenraum (3) der Mahlkammer (50, 51) fördert, dadurch gekennzeichnet, dass das Abtrennsystem aus einem Trennorgan (80, 82) gebildet wird, das zwei koaxial zur Kammerachse (61) angeordnete Kreisscheiben (5, 7) besitzt, zwischen denen mehrere, um den Scheibenmittelpunkt symmetrisch verteilte sowie vom Scheibenrand nach innen führende Förder- bzw. Flügelelemente (12, 86) angeordnet sind, die beim Betrieb der Abtrennvorrichtung einen Gegendruck auf das Gut-Mahlkörper-Gemisch erzeugen, so dass aufgrund der Zentrifugalkraft und der unterschiedlichen spezifischen Dichte die Mahlkörper vom Produkt getrennt und zurück in den Innenraum (3) befördert werden.For fine and fine grinding a good serving, continuously operating horizontal agitator ball mill with a cylindrical or conical, for receiving Mahlkörpern serving grinding chamber (50, 51) one at the end of the grinding chamber (50, 51) arranged and in the interior (3) of the grinding chamber (50, 51) opening Good inlet (37), arranged at the other end of the grinding chamber and out of the interior (3) leading out Good-outlet (38, 39) and a plurality of stirring elements (2) and the chamber axis (60) coaxial agitator (1, 22) and one before the Good outlet (38, 39) arranged separately driven separation system that separates the grinding media from the ground Good and back into the interior (3) of the grinding chamber (50, 51) promotes, characterized in that the separation system is formed by a separating element (80, 82) which has two circular disks (5, 7) arranged coaxially with the chamber axis (61), between which a plurality of disks distributed symmetrically around the disk center point and the disk edge inwardly leading conveying or wing elements (12, 86) are arranged, which generate a back pressure on the material-grinding media mixture during operation of the separating device, so that due to the centrifugal force and the different specific gravity, the grinding media separated from the product and transported back into the interior (3). Rührwerkskugelmühle nach Anspruch 1, dadurch gekennzeichnet, dass die Förder- bzw. Flügelemente bogenförmig sind.Agitator ball mill according to claim 1, characterized in that the conveyor or wing elements are arcuate. Rührwerkskugelmühle nach Ansprüche 2, dadurch gekennzeichnet, dass zusätzlich zu den bogenförmigen Förder- bzw. Flügelelementen (12) auch noch gerade oder annähernd gerade Förder- bzw. Flügelemente (86) vorgesehen sind, die sich vom Scheibenrand nach innen erstrecken.Agitator ball mill according to claim 2, characterized in that in addition to the arcuate conveying or wing elements (12) also straight or approximately straight conveyor or wing elements (86) are provided which extend inwardly from the edge of the disc. Rührwerkskugelmühle nach Anspruch 1, dadurch gekennzeichnet, dass die beiden Kreisscheiben (5, 7) lösbar oder unlösbar miteinander verbunden sind.Agitator ball mill according to claim 1, characterized in that the two circular discs (5, 7) are detachably or permanently connected to each other. Rührwerkskugelmühle nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass zwischen den beiden Kreisscheiben (5, 7) ein mitdrehender Ringkäfig (10) vorgesehen ist, der einen kreisförmigen Hohlraum (8) umschliesst.Agitator ball mill according to claim 1 or 2, characterized in that between the two circular discs (5, 7) a co-rotating ring cage (10) is provided, which encloses a circular cavity (8). Rührwerkskugelmühle nach Anspruch 3, dadurch gekennzeichnet, dass im Ringkäfig (10) ein Siebblechring (6) eingelegt ist.Agitator ball mill according to claim 3, characterized in that in the ring cage (10) a screen plate ring (6) is inserted. Rührwerkskugelmühle nach Anspruch 6, dadurch gekennzeichnet, dass an der Abschlusswand (35) ein Siebabstreifer (65) vorgesehen ist, der dazu dient allenfalls auf dem Sieb festsitzende Mahlkörper und Mahlgut abzustreifen bzw. in Bewegung zu halten.Agitator ball mill according to claim 6, characterized in that on the end wall (35) a Siebabstreifer (65) is provided, which serves at most to strip on the sieve fixed grinding media and ground material or to keep in motion.
EP04405182A 2003-04-15 2004-03-24 Agitator ball mill Revoked EP1468739B1 (en)

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EP2036613A2 (en) 2007-09-13 2009-03-18 Netzsch-Feinmahltechnik GmbH Stirring ball mill
DE102007043670A1 (en) 2007-09-13 2009-04-02 Netzsch-Feinmahltechnik Gmbh stirred ball mill
EP2036613A3 (en) * 2007-09-13 2009-11-25 Netzsch-Feinmahltechnik GmbH Stirring ball mill
US7845589B2 (en) 2007-09-13 2010-12-07 Netzsch-Feinmahltechnik Gmbh Agitating ball mill
TWI410281B (en) * 2007-09-13 2013-10-01 Netzsch Feinmahltechnik Agitating ball mill
EP2106859A3 (en) * 2008-03-31 2014-05-07 Ashizawa Finetech Ltd Media mixing mill
CN101869863B (en) * 2009-04-22 2014-08-13 芦泽精美技术股份有限公司 Media-agitation type pulverizer
US8118247B2 (en) 2009-07-06 2012-02-21 Willy A. Bachofen Ag Agitator ball mill
EP2327480A1 (en) 2009-11-25 2011-06-01 Willy A. Bachofen AG Stirring ball mill
CN102069025B (en) * 2009-11-25 2014-08-20 威利A.巴霍芬股份公司 Agitator ball mill
EP2327479A1 (en) 2009-11-25 2011-06-01 Willy A. Bachofen AG Stirring ball mill
CN102069025A (en) * 2009-11-25 2011-05-25 威利A.巴霍芬股份公司 Agitator ball mill
WO2012055388A3 (en) * 2010-10-27 2012-06-28 Netzsch-Feinmahltechnik Gmbh Stirring ball mill
US8702023B2 (en) 2010-10-27 2014-04-22 Netzch-Feinmahltechnik GmbH Stirring ball mill
WO2012083915A2 (en) 2010-12-04 2012-06-28 Netzsch-Feinmahltechnik Gmbh Dynamic element for the separating device of a stirring ball mill
RU2555915C2 (en) * 2010-12-04 2015-07-10 Неч-Файнмальтехник Гмбх Dynamic element for separator assembly of ball mill with mixer
US8794558B2 (en) 2010-12-04 2014-08-05 Netzsch-Feinmahltechnik Gmbh Dynamic element for the separating device of a stirring ball mill
WO2012083915A3 (en) * 2010-12-04 2012-08-23 Netzsch-Feinmahltechnik Gmbh Dynamic element for the separating device of a stirring ball mill
DE102010053484A1 (en) 2010-12-04 2012-06-06 Netzsch-Feinmahltechnik Gmbh Dynamic element for the separator of a stirred ball mill
US8876028B2 (en) 2010-12-04 2014-11-04 Netzsch-Feinmahltechnik Gmbh Method for operating an agitator ball mill
CN102794215B (en) * 2012-08-21 2016-05-11 向小月 A kind of many circulation grinding system
CN102794215A (en) * 2012-08-21 2012-11-28 向小月 Multi-circulation grinding system
CN102814216A (en) * 2012-08-26 2012-12-12 向小月 Double-shaft grinding system
CN103056011B (en) * 2013-01-24 2016-05-11 陈波 A kind of enforced bidirectional vertical circulation grinding system
CN103056011A (en) * 2013-01-24 2013-04-24 陈波 Forced bi-directional vertical circulation grinding system
US10610871B2 (en) 2013-07-08 2020-04-07 Netzsch-Feinmahltechnik Gmbh Agitator ball mill with axial channels
DE102013111762A1 (en) 2013-07-08 2015-01-08 Netzsch-Feinmahltechnik Gmbh Agitator ball mill with axial channels
WO2015003676A1 (en) 2013-07-08 2015-01-15 Netzsch-Feinmahltechnik Gmbh Stirred ball mill having axial ducts
US11141737B2 (en) 2013-07-08 2021-10-12 Netzsch-Feinmahltechnik Gmbh Agitator ball mill with axial channels
CN103657801A (en) * 2013-12-19 2014-03-26 占天义 Stirring type grinding separator and grinding device
CN103657801B (en) * 2013-12-19 2016-11-23 占天义 Stirring-type grinds separator and lapping device
EP2886198A1 (en) * 2013-12-20 2015-06-24 NETZSCH Trockenmahltechnik GmbH Operating method for a ball mill and ball mill therefor
CN104815726A (en) * 2013-12-20 2015-08-05 耐驰干法研磨技术有限公司 Grinding machine and grinding method thereof
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FR3018807A1 (en) * 2014-03-20 2015-09-25 Herakles PROCESS FOR OBTAINING LOADS OF HEXANITROHEXAAZAISOWURTZITANE CRYSTALS (CL20) OF SUBMICRON SINGLE-MODAL GRANULOMETRY, THE SAID LOADS AND THEIR USE AS SOWING LOADS
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US20050224612A1 (en) 2005-10-13
US7014134B2 (en) 2006-03-21
DE502004006541D1 (en) 2008-04-30
JP2004314066A (en) 2004-11-11
ES2304157T3 (en) 2008-09-16
EP1468739B1 (en) 2008-03-19
DK1468739T3 (en) 2008-07-21
PL1468739T3 (en) 2008-10-31
ATE389456T1 (en) 2008-04-15

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