EP0424490B1 - Procede et dispositif pour produire une poudre de charge propulsive tribasique - Google Patents
Procede et dispositif pour produire une poudre de charge propulsive tribasique Download PDFInfo
- Publication number
- EP0424490B1 EP0424490B1 EP90906180A EP90906180A EP0424490B1 EP 0424490 B1 EP0424490 B1 EP 0424490B1 EP 90906180 A EP90906180 A EP 90906180A EP 90906180 A EP90906180 A EP 90906180A EP 0424490 B1 EP0424490 B1 EP 0424490B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- solvent
- extruder
- powder
- energy carrier
- moist
- 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.)
- Revoked
Links
Classifications
-
- 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
-
- 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
-
- 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
- C06B21/0075—Shaping the mixture by extrusion
Definitions
- the invention relates to a method for producing a three-base propellant charge powder from nitrocellulose, explosive oil and a third, crystalline energy source and additives using a solvent, and to an apparatus for carrying out this method.
- the three-base propellant powders are also known as "cold" powders. Compared to the usual, "hot” powders that do not contain a third, crystalline energy source, they have the advantage of greater protection of the pipe.
- the explosive oil acts as a gelatinator for the nitrocellulose.
- the amount of the explosive oil is often not sufficient for complete gelatinization of the nitrocellulose and a uniform, homogeneous incorporation of the third, crystalline energy carrier into the powder mass, especially if the proportion of the crystalline energy carrier is high.
- three-base propellant powder is produced using an organic solvent as a gelatinization aid.
- the solvent for example a mixture of acetone and alcohol, is added when mixing the raw powder mass and is finally removed from the finished powder.
- a continuously feasible process for the production of three-base propellant powder with solvent has also become known (DE-PS 24 61 646 and US-PS 4,051,207).
- a solvent-moist mixture of all components of the propellant charge powder is pre-plastified on an open, continuously working kneader, ie partially gelatinized.
- the mass usually passes through the kneader several times.
- the pre-plasticized, solvent-containing mass is then gelatinized in an extruder and converted into granulate form.
- the extruder should also be used several times be run through.
- the granules are then pressed in a further extruder to the desired powder strands, which are then cut to length and dried.
- This process is very complex in terms of the necessary mechanical equipment and in the process management, ie the setting and monitoring of the process parameters.
- the invention is based on the object of specifying an improved, continuously executable method of the type mentioned at the outset which, in particular, requires less mechanical effort than previously and the course of which is easily adjustable and controllable.
- a device for performing this method is to be specified.
- Explosive oil in the context of this application is to be understood as the explosive oils usually used for propellant charge powder, in particular nitroglycerin and diglycol dinitrate, as well as mixtures of the aforementioned explosive oils.
- the third, crystalline energy source is usually nitroguanidine (Nigu; NQ).
- nitroguanidine Nigu; NQ
- RDX hexogen
- HMX octogen
- PETN nitropenta
- the additives are those customary in powder production, in particular plasticizers and stabilizers, which are present in the powder mixture in relatively small proportions by weight.
- Drying the powder strands means any measure customary in powder production with which the solvent can be removed from the powder strands practically completely.
- the process according to the invention is characterized in that not all components of the three-base propellant charge powder are mixed with one another from the outset. Rather, a finished gelatinized intermediate product is initially only produced from nitrocellulose and explosive oil, which are premixed into a water-moist raw mass, in a single pass on an open kneading device without the use of solvent.
- This gelatinized and therefore dry intermediate product is granulated and fed as granules together with the third, crystalline energy source to a closed extruder, the solvent being added only now. Kneading in a closed extruder creates a homogeneous, doughy mass in which the crystalline energy source is uniformly and finely distributed. This solvent-moist mass is extruded from the kneading into powder strands in the same extruder, which are then cut to length and dried in the usual manner.
- the method according to the invention can be carried out continuously. To carry it out, it only requires two essential machines, namely the open kneading device and the closed extruder, in addition a pelletizing device downstream of the open kneading device and a means for transporting the pellets to the extruder.
- the procedure is simple. Each machine only needs to be run once. Even if the recipes are changed frequently, it is not difficult to adjust the respective process parameters in a new and correct manner and to monitor their compliance.
- An advantage in this context is the fact that the first part of the process, the processing of the raw mass on the open kneading device, runs little differently than in the usual production of dibasic propellant powders, so that the routines and experience of this production method can be used in this respect .
- This also guarantees a high level of security.
- the nitrocellulose is completely gelatinized by the Explosive oil is particularly at high risk of self-ignition of the powder mass in every production, for example due to excretion of explosive oil from the raw mass.
- the method according to the invention only works on the open kneading device, where the consequences of any self-ignition are far more harmless than in a closed processing device, for example an extruder.
- the risk of explosion is significantly reduced by the addition of the solvent in the process according to the invention.
- the method according to the invention manages with a significantly smaller amount than the solvent in terms of the production volume than the conventional manufacturing method and the losses of solvent during drying of the extruded powder strands are correspondingly lower, which increases the economy and makes a contribution to environmental protection. For the same reason, the drying effort compared to the usual method is considerably lower.
- a shear roller mill which is known per se for the homogenization and plasticization of non-explosive thermoplastic materials, for example plastics, is preferably used as the open kneading device (EP-A 0 148 966 or US Pat. No. 4,605,309).
- the shear roller mill has two independently drivable rollers, between which there is an adjustable roller gap.
- the rollers are provided with spiral grooves, which ensure that the processed material is securely drawn into the gap and at the same time generate an axial transport movement in the nip from one end of the pair of rollers to the other end.
- the water-moist raw mass is continuously fed onto the two rollers of the shear roller mill at one end and then gradually transported to the other end of the two rollers with kneading and intensive shearing.
- the raw material arriving at the other end is then gelatinized.
- the water must be removed from the raw mass. This is done by squeezing in the roller gap and also by evaporating the water, since the rollers of the shear roller mill are heated.
- the raw powder mass fed to the shear roller mill preferably has a water moisture content of 20% to 30%. The removal of this water and thus the increasing gelatinization of the raw material takes place gradually during the migration of the raw material along the rollers.
- the process can be controlled in such a way that the raw mass at the discharge end of the roller pair is practically dry and thus gelatinized, which means that the residual water content is less than 3% and preferably less than 1%, for example 0.5%.
- the finished gelatinized raw material is located on one of the two rollers and can be removed there continuously with simultaneous granulation, for example with a granulating head.
- the process according to the invention also has the advantage that the recipes can be adhered to very precisely and the production of various propellant powders can therefore be reproduced exactly because Both the intermediate product due to its granular form and the third crystalline energy source can both be fed to the extruder in precisely metered form, for example with the aid of suitable metering devices.
- the extruder requires a first filling opening for the granules in the working direction, then an opening for the supply of the solvent and then an opening for the supply of the crystalline energy source under pressure, which is technically somewhat more complex.
- the additives can already be fed to the kneading device together with the premixed water-moist raw material.
- the joint application of both options can be done in In individual cases, ie depending on the particular recipe, it may be useful, for example, in such a way that certain additives are only fed to the kneading device and the remaining additives to the extruder.
- the raw mass fed to the shear roller usually comprises 40% to 60% and preferably 45% to 55% nitrocellulose.
- the crystalline energy source is metered into the extruder in an amount of 10% to 55% and preferably in an amount between 40% and 55% of the granules supplied.
- the solvent is expediently fed to the extruder in an amount of 60 to 130 grams per kilogram of the solids fed (granules + crystalline energy source). This means a saving in solvent of 30% to 60% compared to conventional manufacturing processes.
- solvents are Alcohol or acetone in question. The selection depends, among other things. on the degree of nitration of the nitrocellulose used. The higher the degree of nitration, the more or the sharper the solvent is generally necessary.
- a device for carrying out the method according to the invention is characterized by an open shear roller mill, a downstream granulating device, a transport device and a closed extruder.
- the device shown comprises an open shear roller mill 1, as is known, for example, from US Pat. No. 4,605,309.
- the shear roller mill has two independently drivable rollers, between which a roller gap is formed.
- the pre-mixed, water-moist raw powder mixture of water-moist nitrocellulose and explosive oil is fed to the shear roller mill.
- the feed is indicated in the drawing by a feed hopper and an arrow.
- the raw mass is kneaded in the shear roller mill and thereby gelatinized while removing the water.
- a pelletizing device 2 is assigned to this end of the two rolls, with which the gelatinized raw material or the intermediate product is removed from one of the two rolls and thereby pelletized.
- the granulated intermediate product reaches the input opening 5 of a closed extruder 4 by means of a transport device 3.
- the third, crystalline energy carrier is fed to the same input opening 5.
- the granulate and the third energy carrier are expediently supplied in each case via a metering device (not shown in more detail).
- an addition device 6 is provided on the extruder 4 for the addition of solvent.
- a further filling opening 7 can be provided behind the feed device 6, via which the crystalline energy carrier is introduced into the extruder separately from the granulate. This must then be done under pressure because a pressure has already built up in the area of the filling opening 7 inside the extruder.
- the extruder 4 is provided in the usual way with one or two screws 8, which are rotatably mounted in the housing of the extruder and are only indicated schematically here.
- a die not shown
- the material is extruded into powder strands.
- the solvent e.g. Alcohol
- This solvent-containing mass is finally passed through the die of the extruder e.g. extruded into a 7-hole powder strand.
- the powder strands emerging from the extruder are cut to length in a conventional manner, not shown, and suitably, e.g. in a drying facility, freed from the solvent.
- the two rollers of the shear roller mill can be heated to temperatures between 80 o C and 120 o C.
- the adjustable speed range of the two rollers is between 40 and 70 rpm.
- the gap between the two rollers is usually set to less than 2 mm .
- the granulating device 2 delivers a granulate in the size of 3 to 6 mm.
- the extruder 4 is typically designed with a length to diameter ratio of 20 to 24.
- the temperature inside is between 20 o C and 50 o C.
- the screw speed can be set between 30 and 80 rpm.
- the dry granules and nitroguanidine as the third energy source are metered into the extruder in a weight ratio of 45% granules and 55% nitroguanidine, where they are homogenized with the aid of solvents and extruded into a 7-hole powder.
- the throughput here is 40 kilograms per hour at a screw speed of 60 rpm and an extruder head pressure of 23 bar.
- a mixed raw mass of 62% nitrocellulose, 37% nitroglycerin, 0.3% centralite, 0.5% acardite, 0.1% magnesium oxide and 0.1% graphite with an initial water content is placed on the shear roller mill 1 processed by 28%.
- the temperature of the first roller is 110 ° C. and its speed is 50 rpm, the temperature the second roller 90 o C and its speed 45 rpm. This results in a throughput of 42 kilograms of dry mass per hour with a water content of approx. 0.7% at the granulating device.
- the granules and nitroguanidine are metered into the extruder in a weight ratio of 60%: 40% and processed there with acetone as solvent in an amount of 3 liters per hour and extruded to form a 7-hole bulk powder.
- the screw speed is 40 rpm
- the head pressure is 27 bar
- the head temperature is 48 o C.
- the throughput is 30 kg per hour.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Medicinal Preparation (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Glanulating (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Formation And Processing Of Food Products (AREA)
Abstract
Claims (9)
- Procédé pour la fabrication d'une poudre tribasique de charge propulsive à partir de nitrocellulose, d'huile explosive et d'un troisième vecteur d'énergie cristallin ainsi que d'additifs, en utilisant un solvant, caractérisé par les étapes suivantes :a) la masse brute humectée d'eau prémélangée à partir de nitrocellulose humectée d'eau et d'huile explosive est gélatinisée sur un dispositif malaxeur ouvert travaillant en continu et est en même temps séchée, le processus de malaxage étant réglé de manière que la masse brute au moment de quitter le dispositif malaxeur soit transformée en un produit intermédiaire gélatinisé avec une teneur résiduelle en eau inférieure à 3 % ;b) le produit intermédiaire est transformé en granulat au moment de quitter le dispositif malaxeur ;c) le produit intermédiaire granulé (granulat) et le troisième vecteur d'énergie cristallin ainsi que le solvant sont amenés à une extrudeuse fermée travaillant en continu pour y être homogénéisés par malaxage et être extrudés sous forme de barres de poudre humectées de solvant, auquel cas on mélange, dans le sens de travail de l'extrudeuse, tout d'abord le granulat et le vecteur d'énergie cristallin et ensuite le solvant ;d) les barres de poudres humectées de solvant sont coupées à la longueur et séchées.
- Procédé selon la revendication 1,
caractérisé en ce qu'
un laminoir broyeur ouvert à cylindres est utilisé comme dispositif malaxeur. - Procédé selon la revendication 1 ou 2,
caractérisé en ce que
les additifs sont délivrés, ensemble avec la masse brute prémélangée humectée en eau, au dispositif malaxeur. - Procédé selon la revendication 1, 2 ou 3,
caractérisé en ce que
les additifs sont délivrés, ensemble avec le granulat et le troisième vecteur d'énergie cristallin, à l'extrudeuse. - Procédé selon l'une des revendications 1 à 4,
caractérisé en ce que
la masse brute amenée au cylindre broyeur comprend 40 % à 60 % de nitrocellulose. - Procédé selon l'une des revendications 1 à 5,
caractérisé en ce que
la masse brute amenée au cylindre broyeur présente une humidité de 20 % à 30 %. - Procédé selon l'une des revendications 1 à 6,
caractérisé en ce que
le vecteur d'énergie cristallin est délivré à l'extrudeuse dans une proportion de 10 % à 55 % du granulat fourni. - Procédé selon l'une des revendications 1 à 7,
caractérisé en ce que
le solvant est amené à l'extrudeuse dans une proportion de 60 à 130 g par kg de matière solide fournie (granulat + vecteur d'énergie cristallin). - Dispositif pour la mise en oeuvre du procédé selon l'une des revendications 1 à 8,
caractérisé par
un laminoir broyeur ouvert à cylindres, un dispositif de granulation placé après, un dispositif de transport et une extrudeuse fermée qui présente une première ouverture de remplissage dans le sens de travail pour le granulat et le vecteur d'énergie cristallin et ensuite une ouverture pour l'amenée du solvant.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3915437 | 1989-05-11 | ||
DE3915437 | 1989-05-11 | ||
PCT/EP1990/000616 WO1990013528A2 (fr) | 1989-05-11 | 1990-04-17 | Procede et dispositif pour produire une poudre de charge propulsive tribasique |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0424490A1 EP0424490A1 (fr) | 1991-05-02 |
EP0424490B1 true EP0424490B1 (fr) | 1995-03-08 |
Family
ID=6380472
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP90906180A Revoked EP0424490B1 (fr) | 1989-05-11 | 1990-04-17 | Procede et dispositif pour produire une poudre de charge propulsive tribasique |
Country Status (19)
Country | Link |
---|---|
US (1) | US5266242A (fr) |
EP (1) | EP0424490B1 (fr) |
JP (1) | JPH0777992B2 (fr) |
KR (1) | KR940004634B1 (fr) |
CN (1) | CN1042324C (fr) |
AR (1) | AR242765A1 (fr) |
AT (1) | ATE119512T1 (fr) |
AU (1) | AU632562B2 (fr) |
BR (1) | BR9006751A (fr) |
CA (1) | CA2031517C (fr) |
DE (1) | DE59008631D1 (fr) |
EG (1) | EG21067A (fr) |
FI (1) | FI97802C (fr) |
GR (1) | GR1003566B (fr) |
IL (1) | IL94193A (fr) |
NO (1) | NO175936C (fr) |
PT (1) | PT94013A (fr) |
WO (1) | WO1990013528A2 (fr) |
ZA (1) | ZA903514B (fr) |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SE501223C2 (sv) * | 1992-08-28 | 1994-12-12 | Bofors Explosives Ab | Sätt och anordning för att framställa pyrotekniska satser genom valsning |
US5487851A (en) * | 1993-12-20 | 1996-01-30 | Thiokol Corporation | Composite gun propellant processing technique |
FR2723086B1 (fr) * | 1994-07-29 | 1996-09-13 | Poudres & Explosifs Ste Nale | Procede continu de fabrication sans solvant de produits pyrotechniques composites |
WO1998042640A1 (fr) | 1997-03-21 | 1998-10-01 | Cordant Technologies, Inc. | Procede de fabrication de poudre noire et de substitut de poudre noire |
ATE298736T1 (de) | 1999-02-23 | 2005-07-15 | Gen Dynamics Ordnance & Tactic | Perforierter treibstoff und verfahren zu seiner herstellung |
US6315930B1 (en) | 1999-09-24 | 2001-11-13 | Autoliv Asp, Inc. | Method for making a propellant having a relatively low burn rate exponent and high gas yield for use in a vehicle inflator |
DE102010020776B4 (de) * | 2010-05-18 | 2015-03-05 | Diehl Bgt Defence Gmbh & Co. Kg | Treibladung und Verfahren zu ihrer Herstellung |
CN102826942B (zh) * | 2012-09-18 | 2013-07-31 | 湖南省浏阳金生花炮有限公司 | 一种无烟烟花发射药 |
US9539752B2 (en) * | 2013-08-09 | 2017-01-10 | General Dynamics Ordnance and Tactical Systems—Canada Valleyfield, Inc. | Continuous celluloid twin screw extrusion process |
CN103980071A (zh) * | 2014-05-06 | 2014-08-13 | 西安近代化学研究所 | 一种用于炸药捏合碾片的滚筒装置 |
JP6472628B2 (ja) * | 2014-09-30 | 2019-02-20 | カーリットホールディングス株式会社 | 液体推進薬の製造方法 |
CN104950056B (zh) * | 2015-07-14 | 2017-03-01 | 西安近代化学研究所 | 一种叠氮硝胺吸收药样品制备方法 |
CN105367360B (zh) * | 2015-12-28 | 2017-09-29 | 中国科学院沈阳自动化研究所 | 一种制备炮弹发射药自动上料装置 |
CN110540484B (zh) * | 2019-10-14 | 2021-06-15 | 北方化学工业股份有限公司 | 一种烟花用硝化棉连续制备工艺 |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3086896A (en) * | 1961-01-19 | 1963-04-23 | Russell L Trask | Nitroguanidine propellant composition and process of preparation |
DE2316538C3 (de) * | 1973-04-03 | 1982-05-06 | Dynamit Nobel Ag, 5210 Troisdorf | Verfahren zur Herstellung von Gudol- Pulver |
US4076773A (en) * | 1974-11-25 | 1978-02-28 | W. R. Grace & Co. | Process for prilling ammonium nitrate |
DE2461646C2 (de) * | 1974-12-27 | 1984-01-05 | Dynamit Nobel Ag, 5210 Troisdorf | Verfahren zur Herstellung von Treibladungspulvern |
DE2825567B1 (de) * | 1978-06-10 | 1979-11-15 | Dynamit Nobel Ag | Verfahren zur kontinuierlichen Herstellung von Explosivstoffgemischen |
DE2900020C2 (de) * | 1979-01-02 | 1982-12-09 | WNC-Nitrochemie GmbH, 8261 Aschau | Verfahren zur Herstellung eines mehrbasigen Treibladungspulvers |
NO144666C (no) * | 1980-02-29 | 1981-10-14 | Dyno Industrier As | Fremgangsmaate for fremstilling av aluminiumholdige hoeyenergisprengstoffblandinger |
DE3042697C2 (de) * | 1980-11-12 | 1986-02-20 | WNC-Nitrochemie GmbH, 8261 Aschau | Verfahren zum kontinuierlichen Herstellen einbasiger Pulver |
DE3242301A1 (de) * | 1982-11-16 | 1984-05-17 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V., 8000 München | Verfahren und vorrichtung zur herstellung ein- oder mehrbasiger treibladungspulver |
US4726919A (en) * | 1985-05-06 | 1988-02-23 | Morton Thiokol, Inc. | Method of preparing a non-feathering nitramine propellant |
US4650617A (en) * | 1985-06-26 | 1987-03-17 | Morton Thiokol Inc. | Solvent-free preparation of gun propellant formulations |
DE3532525A1 (de) * | 1985-09-12 | 1987-03-19 | Fraunhofer Ges Forschung | Dreibasiges treibladungspulver und verfahren zu seiner herstellung |
DE3635296C2 (de) * | 1986-10-16 | 1995-12-21 | Nitrochemie Gmbh | Verfahren zum Herstellen von Treibladungspulver |
-
1990
- 1990-04-17 WO PCT/EP1990/000616 patent/WO1990013528A2/fr not_active Application Discontinuation
- 1990-04-17 CA CA002031517A patent/CA2031517C/fr not_active Expired - Fee Related
- 1990-04-17 KR KR1019910700035A patent/KR940004634B1/ko not_active IP Right Cessation
- 1990-04-17 US US07/635,169 patent/US5266242A/en not_active Expired - Lifetime
- 1990-04-17 BR BR909006751A patent/BR9006751A/pt not_active IP Right Cessation
- 1990-04-17 DE DE59008631T patent/DE59008631D1/de not_active Expired - Fee Related
- 1990-04-17 EP EP90906180A patent/EP0424490B1/fr not_active Revoked
- 1990-04-17 JP JP2505966A patent/JPH0777992B2/ja not_active Expired - Fee Related
- 1990-04-17 AU AU54244/90A patent/AU632562B2/en not_active Ceased
- 1990-04-17 AT AT90906180T patent/ATE119512T1/de not_active IP Right Cessation
- 1990-04-23 GR GR900100307A patent/GR1003566B/el not_active IP Right Cessation
- 1990-04-24 IL IL9419390A patent/IL94193A/en not_active IP Right Cessation
- 1990-05-02 AR AR90316761A patent/AR242765A1/es active
- 1990-05-09 ZA ZA903514A patent/ZA903514B/xx unknown
- 1990-05-09 EG EG27290A patent/EG21067A/xx active
- 1990-05-10 CN CN90102643A patent/CN1042324C/zh not_active Expired - Fee Related
- 1990-05-11 PT PT94013A patent/PT94013A/pt not_active Application Discontinuation
- 1990-12-28 FI FI906423A patent/FI97802C/fi not_active IP Right Cessation
-
1991
- 1991-01-11 NO NO910139A patent/NO175936C/no not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
FI97802C (fi) | 1997-02-25 |
EG21067A (en) | 2000-10-31 |
CA2031517A1 (fr) | 1990-11-12 |
ZA903514B (en) | 1991-02-27 |
CA2031517C (fr) | 1999-08-24 |
KR920701080A (ko) | 1992-08-11 |
PT94013A (pt) | 1991-01-08 |
BR9006751A (pt) | 1991-08-06 |
AR242765A1 (es) | 1993-05-31 |
GR900100307A (el) | 1991-10-10 |
DE59008631D1 (de) | 1995-04-13 |
EP0424490A1 (fr) | 1991-05-02 |
FI906423A0 (fi) | 1990-12-28 |
ATE119512T1 (de) | 1995-03-15 |
WO1990013528A2 (fr) | 1990-11-15 |
US5266242A (en) | 1993-11-30 |
IL94193A0 (en) | 1991-01-31 |
GR1003566B (el) | 2001-04-10 |
AU632562B2 (en) | 1993-01-07 |
WO1990013528A3 (fr) | 1990-12-27 |
JPH03505199A (ja) | 1991-11-14 |
AU5424490A (en) | 1990-11-29 |
CN1042324C (zh) | 1999-03-03 |
CN1047072A (zh) | 1990-11-21 |
IL94193A (en) | 1994-11-28 |
NO175936B (no) | 1994-09-26 |
NO910139D0 (no) | 1991-01-11 |
FI97802B (fi) | 1996-11-15 |
JPH0777992B2 (ja) | 1995-08-23 |
NO175936C (no) | 1995-01-04 |
KR940004634B1 (ko) | 1994-05-27 |
NO910139L (no) | 1991-01-11 |
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