EP1110687B2 - Procédé de production d'un panneau de fibres léger à surface fermée - Google Patents
Procédé de production d'un panneau de fibres léger à surface fermée Download PDFInfo
- Publication number
- EP1110687B2 EP1110687B2 EP00124199A EP00124199A EP1110687B2 EP 1110687 B2 EP1110687 B2 EP 1110687B2 EP 00124199 A EP00124199 A EP 00124199A EP 00124199 A EP00124199 A EP 00124199A EP 1110687 B2 EP1110687 B2 EP 1110687B2
- Authority
- EP
- European Patent Office
- Prior art keywords
- binder
- bulk density
- fibres
- fibers
- fibre
- 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.)
- Expired - Lifetime
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/005—Manufacture of substantially flat articles, e.g. boards, from particles or fibres and foam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
Definitions
- the individual wood fibers shrink to each other, unless a binder is used. If a binder is used, so that it is in the known method to such a according to the preamble of claim 1, it is important to ensure that the binder is fixed to the wood fibers, since it is otherwise aspirated with the water of the starting suspension or is squeezed.
- the fiberboards obtained by the known wet process may have the desired low density. But they have a loose open surface, which is not very suitable for many applications on. For example, fiber boards produced by the wet process which are used as insulation panels in interior construction can not readily be papered or otherwise coated with thin materials.
- a so-called dry process for the production of fiberboards from lignocellulosic fibers and binders is known.
- the fibers are obtained in the same way as for the wet process. Subsequently, however, they are not transferred into a suspension, but dried in current dryers, ie in flight, to a level that later allows easier removal of the residual moisture.
- the residual moisture content of the fibers after drying is less than 20%, typically less than 10%.
- a binder is added to the fibers, which, after the subsequent shaping of the fibers into a fiber mat during hot pressing of the fiber mat between pressure-controlled heating surfaces to a fiberboard, glues the individual fibers together.
- a process for producing fiberboard which is also to be arranged between a true wet process and a dry process.
- fibreboards with a low density of up to well below 150 kg / m 3 , allegedly down to 60 kg / m 3 can be produced.
- fibers made of wood are mixed with a binder and applied to a forming station with a spreader to form a fiber mat.
- the fiber mat is precalibrated in width and basis weight and shaped and cured after activation of the binder by a heat treatment to form the fiberboard.
- the activation of the binder should be done for example by steam. To harden the fiber mat, this is to be flowed through with a drying medium, for example with hot air. If a thickness formation takes place in a press, the pressing surfaces should be designed like a sieve. In this way, as in a wet process, fiber plates with open and produced by the screen surfaces used structured surface, which also have all the disadvantages of known produced in the wet process fiberboard.
- the DE 198 18 879 A1 discloses a method and apparatus for the continuous production of fiberboard. The production of ultralightweight plates with a density of less than or equal to 400 kg / m 3 is also described. That from the DE 195 18 879 A1 known method is characterized in that after the pre-compression of the fiber mat in the inlet gap in the following main press sections of a hot press by means of flexible press racks and / or press segments decompressing or compressing a low-pressure zone with a steep slope or fall angle for a vertical stroke of 0 to about 10 mm increasing extremely short at maximum production speed during production can be controlled. In Fig.
- the invention has for its object to provide a method for producing lightweight fiberboard according to the preamble of claim 1, which is simple and economical to carry out and yet leads to fiberboard with improved surface properties.
- the new process is a dry process because the fiber moisture content of the fibers is less than 20% when calibrating the fiber mat and during the heat treatment to cure the binder. It can be in the range below 10% as with conventional dry processes.
- the heat treatment of the fiber mat via smooth closed heating surfaces, via which the heat is transferred to the curing of the binder on the fiber mat. It is important that the heating surfaces are distance-controlled and not pressure-controlled, as is the case when carrying out conventional drying processes.
- the very low bulk density of the fiber boards produced by the new process does not allow controlled pressure control of the heating surfaces.
- the fiber mat before the heat treatment it is preferable to use the fiber mat before the heat treatment to spray with water or an aqueous solution.
- a jet of steam can be directed into the interior of the fiber mat, which promotes the curing of the binder there.
- the water softens the fibers on the surface of the fiber mat, so that can be achieved by the action of smooth heating surfaces particularly good smooth surfaces in the finished fiberboard.
- the fiber mat can also be calibrated by the heating surfaces controlled at a distance.
- the predetermined distance of the heating surfaces which corresponds to the thickness of the fiberboard produced, is typically 20 to 300 mm. It is amazing, especially in the area of larger thicknesses in this area, that the fibreboards can nevertheless be produced by a dry process.
- the density profile of the fiberboard is adjusted so that there is an edge overshoot of the density compared to the average density of the fiberboard of at least 60%.
- a stronger edge increase of the bulk density is the basis for the formation of a particularly strong closed surface of the finished fiberboard, which may for example also have a considerable pressure stability compared to the average bulk density of the fiberboard.
- a common synthetic resin of the wood-based material industry can be used as the binder.
- the usual synthetic resins of the wood-based materials industry include urea-formaldehyde, melamine-urea-formaldehyde, melamine-urea-phenol-formaldehyde, phenol-urea-formaldehyde, phenol-formaldehyde and PMDI resins.
- a foaming polyurethane binder may be used as the binder.
- the advantage of filling the voids in the fiberboard between the individual fibers by the polyurethane foam is no longer noticeable in an economically utilizable way.
- the particularly light fiberboard in the range below 150 kg / m 3 but can not be produced in usable quality without the use of a foam-forming binder.
- foam-forming polyurethane binder As a foam-forming polyurethane binder, a so-called one-component system can be used, which was developed for example by Bayer and is basically available. Preferably, however, an easily controllable two-component system is used, wherein the foam-forming polyurethane binder comprises a first, NCO group-containing binder component and a second at least one polyol having binder component.
- the relevant main part of the polyurethane reaction is triggered, which then leads to the desired binding of the fibers in the fiberboard. It is surprising that, in spite of the microscopically inhomogeneous distribution of the binder components in the heat treatment, the polyurethane reaction finally takes place completely. That is, there is no noticeable reaction loss due to the fact that both binder components are not present on all fibers. At the same time, since the reactivity of the binder is fully concentrated on the polyurethane reaction within the fiber mat, the binder can be used in relatively small proportions based on the fibers and the desired strength of the fiberboard.
- the first batch may in principle contain 10 to 90% and the second batch corresponding to 90 to 10% of the total fibers. But it makes sense if the first and the second part of the fibers are about the same size, d. H. For example, each contain 40 to 60% of the total fibers.
- the novel process can be carried out both batchwise and continuously, which is preferred.
- the heating surfaces are typically provided on rear-heated metal endless belts.
- the lots can of the fibers are stored separately after application of the binder components and prior to their mixing.
- the reactivity of the binder components does not decrease even with prolonged periods of separate storage of the batches of fibers.
- the heat treatment can be carried out so that in the middle of the molded body, a temperature of only 50 to 100 ° C is reached. This means that in comparison to known methods very low temperatures in the middle of the molding are sufficient. Conversely, these result in a high efficiency of the energy used in the heat treatment and short periods of time required for the heat treatment.
- the low temperature is sufficient in the new process at least for curing the binder content in the middle of the molding, if highly reactive polyurethane binders are used whose reaction is not chemically hindered to suppress a pre-reaction.
- the fibers processed in the new process are wood fibers in the form of conventional defibrator pulp.
- the binder content can be selected within the limits of the new process, which are set by the necessary strength of the fiberboard on the one hand and the economy of the process face high binder costs on the other hand.
- the following information refers to the use of a polyurethane binder.
- the average density of the shaped body is adjusted to 60 to 250 kg per m 3 , wherein the binder content of the molding is adjusted to a total of 2.5 to 5% by weight based on atro wood fibers.
- the average density of the molding is adjusted to 250 to 400 kg / m 3 , wherein the binder content of the molding is adjusted to a total of 7 to 15% by weight based on atro wood fibers.
- the novel process may also be carried out by forming a layered structure having different compositions and / or proportions of the binder in the individual layers as the preform is formed from the fibers.
- the binder components in the cover layers of a fiberboard can be larger than in the middle layer in order to achieve a particularly high stability of the cover layers.
- mechanically stable fiberboards result using a foam-forming binder, ie a polyurethane binder which has at least two binder components PMDI and polyol or which is a one-component system.
- a foam-forming binder ie a polyurethane binder which has at least two binder components PMDI and polyol or which is a one-component system.
- Such fiber boards may also be considered fiber stabilized polyurethane foam.
- the binder content of atro fibers is at least 5%, so in absolute terms it is still relatively small.
- binder content can be reduced when using a foam-forming polyurethane binder below 5% atro fibers. If the stabilities are not paramount, binder levels down to within 1% may be sufficient. All percentages are, as usual, weight percentages.
- binder content should also be selected for lower strengths above 5%, and for higher strengths 7 to 15% binder content should be used.
- a foam-forming binder can be used, in which case high-strength fiberboard can be produced even with relatively low binder levels.
- the method shown in the flow chart according to the figure for producing polyurethane-bonded molded body is based on wood 1, which is comminuted in the usual way and then digested in a defibrator 2 in individual wood fibers 3.
- the stream of wood fibers 3 is then divided into an allocation device 4 in two lots 5 and 6, the lots 5 and 6 are the same size.
- an NCO-group-containing binder component 8 a so-called PMDI, is applied in an application device 7.
- the formulation of the PMDI 8 corresponds to one that is commonly used as the sole binder in the wood-based panel industry.
- an at least one polyol-containing binder component 10 is applied in an applicator 9.
- This is preferably a mixture of a short-chain and a long-chain polyol.
- a mixture of one part of diethylene glycol and one part of 1000 molar mass of polyether alcohol can be used.
- Both applicators 7 and 9 operate on the principle that the PMDI 8 and the polyol 10 is sprayed onto the wood fibers 3.
- the batches 5 and 6 are temporarily stored in separate buffers 11 and 12 if necessary. These may be conventional wood fiber bunkers.
- An intermediate storage is basically optional and does not necessarily have to be done. However, it makes it possible to decouple the further method steps from the method steps described so far in order ultimately to achieve an optimum efficiency of the production method.
- a mixing device 13 the wood fibers 3 of the lots 5 and 6 are mixed together.
- the required mixing can also be done by rolling a scattering head of a spreader 14. From the wood fibers 3 of both lots 5 and 6, a fiber mat 15 is scattered in the scattering device 14, which represents a preform of the fiber boards 18 produced here.
- the fiber mat 15 is calibrated in a calibration device 16, which is a cold precompacting prepress.
- a hot press 17 a heat treatment, from which the desired fiberboard 18 results.
- the hot press 17 is not to be understood that the fiber mat 15 is necessarily compressed with the application of pressure. Rather, the plates of the hot press 17 are distance-controlled, in order to come to the fiber mat 18 with a defined thickness even without lasting back pressure of the fiber mat 15.
- the new process can be carried out both with a belt press as hot press 17 and with a discontinuous hot press. It may be advantageous to provide hot air heating or high frequency heating of the calibrated fiber mat 15 instead of or alternatively to hot contact surfaces. When heating via hot contact surfaces, it is advantageous to spray the surfaces of the fiber mat 15 with water, so that the evaporating at the hot contact surfaces water also transfers heat into the interior of the fiber mat 15. This is particularly advantageous when the fiber mat 15 is very thick, d. H. more than 40 mm thick.
- the PMDI used i. H. the binder component having NCO groups, a composition as is customary in the wood-based panel industry.
- the second, polyol-containing binder component was also already mentioned above mixture of one part of diethylene glycol and one part of polyether alcohol of molecular weight 1000.
- a mixing device 13 a simple rotary drum was used.
- the mixing time of the two games 5 and 6 was 10 seconds.
- the temperature of the contact surfaces of the hot press 17 was set at 170 ° C. All% values are in% by weight.
- the PMDI 8 was used in a proportion of 2.5% and the polyol 10 in a proportion of 1% based on atro wood fibers 3. After 240 sec. Dwell time of the fiber mat 15 in the hot press 17 was a 100 mm thick fiber plate 18 removed. The average bulk density of this fiberboard 18 was 80 kg / m 3 . Despite the very low compression of the wood fibers in this fiber board, the fiber board for an insulating material was perfectly stable and manageable.
- the binder proportions corresponded to Example 1. After 300 sec. Dwell time of the fiber mat 15 in the hot press 17, a 50 mm thick fiber plate 18 was removed. The average bulk density was 170 kg / m 3 . The flexural strength of the fiberboard 18 was 0.3 N / mm 2 . The compressive stress at 10% compression was 0.18 N / m 2 .
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Dry Formation Of Fiberboard And The Like (AREA)
- Laminated Bodies (AREA)
Claims (14)
- Procédé de fabrication de panneaux de fibres légers d'une masse volumique apparente médiane de 60 à 350 kg/m3 à base de fibres sous forme de bois désintégré dans un défibreur en fibres de bois séparées contenant de la lignocellulose, et d'un liant, le liant étant appliqué sur les fibres et les fibres étant formées ensuite en un mat de fibres qui est calibré et soumis à un traitement thermique pour durcir le liant, caractérisé en ce qu'on règle une humidité des fibres (3) telle que lors du calibrage du mat de fibres (15) et du traitement thermique elle soit inférieure à 20 %, et en ce que le mat de fibres (15) est mis en contact, lors du traitement thermique pour le transfert de chaleur, sur les deux faces avec des surfaces chauffantes fermées lisses, les surfaces chauffantes opposées l'une à l'autre étant commandées avec un écartement pour respecter une distance prédéfinie, et un profil de la masse volumique apparente des panneaux des fibres (18) étant réglé de manière à obtenir une masse volumique apparente sur les bords supérieure d'au moins 20 % à la masse volumique apparente médiane des panneaux de fibres (18).
- Procédé selon la revendication 1, caractérisé en ce qu'on pulvérise de l'eau ou une solution aqueuse avant le traitement thermique sur le mat de fibres (15).
- Procédé selon la revendication 1 ou 2, caractérisé en ce que la distance prédéfinie des surfaces chauffantes est comprise entre 20 et 300 mm.
- Procédé selon l'une des revendications 1 à 3, caractérisé en ce que le profil de masse volumique apparente des panneaux de fibres (18) est réglé de manière à obtenir une masse volumique apparente supérieure d'au moins 60 % à la masse volumique apparente médiane des panneaux de fibres.
- Procédé selon l'une des revendications 1 à 4, caractérisé en ce que la masse volumique apparente médiane des panneaux de fibres (18) est réglée de 150 à 350 kg/m3, une résine synthétique usuelle de l'industrie des matériaux de bois étant utilisée comme liant (8, 10), dans le groupe qui comprend des résine UF, MUF, MUPF, PUF, PF et PMDI.
- Procédé selon l'une des revendications 1 à 4, caractérisé en ce que la masse volumique apparente médiane des panneaux de fibre (18) est réglée de 60 à 250 kg/m3, un liant PUR formant une mousse étant utilisé comme liant (8, 10).
- Procédé selon la revendication 6, caractérisé en ce que le liant PUR formant une mousse contient un premier composant de liant (8) comportant des groupes NCO ainsi qu'un deuxième composant de liant (9) comprenant au moins un polyol.
- Procédé selon la revendication 7, caractérisé en ce que les fibres sont divisées en au moins deux parties (5, 6) avant l'application du liant (8,9), en ce que sur une première (5) de ces parties on n'applique que le premier composant de liant (8) comportant des groupes NCO, et sur une deuxième (6) de ces parties, que le deuxième composant de liant (9) comportant le polyol, et en ce que les parties (5, 6) des fibres (3) sont mélangées entre elles avant le formage du mat de fibres (15).
- Procédé selon la revendication 8, caractérisé en ce que la première partie (5) contient de 10 à 90 % et la deuxième partie (6) de 90 à 10 % des fibres (3) totales.
- Procédé selon la revendication 9, caractérisé en ce que la première partie (5) contient de 40 à 60 % et la deuxième partie (6) de 60 à 40 % des fibres (3) totales.
- Procédé selon l'une des revendications 8 à 10, caractérisé en ce que sur une troisième partie des fibres (3) on n'applique aucun composant du liant avant le mélange.
- Procédé selon l'une des revendications 1 à 11, caractérisé en ce que le procédé est mis en oeuvre de façon continue.
- Procédé selon l'une des revendications 1 à 12, caractérisé en ce que le traitement thermique est exécuté jusqu'à ce que soit atteinte une température de 50 à 100 °C au milieu du mat de fibre (15).
- Procédé selon l'une des revendications 1 à 13, caractérisé en ce que lors du formage du mat de fibres (15) à partir des fibres (3), on règle une constitution en couches avec différentes compositions et / ou proportions du liant dans les différentes couches.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19963096 | 1999-12-24 | ||
DE19963096A DE19963096C1 (de) | 1999-12-24 | 1999-12-24 | Verfahren zur Herstellung Polyurethan-gebundener Formkörper aus Lignocellulose-haltigen Partikeln |
Publications (3)
Publication Number | Publication Date |
---|---|
EP1110687A1 EP1110687A1 (fr) | 2001-06-27 |
EP1110687B1 EP1110687B1 (fr) | 2005-12-21 |
EP1110687B2 true EP1110687B2 (fr) | 2010-02-03 |
Family
ID=7934563
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00124199A Expired - Lifetime EP1110687B2 (fr) | 1999-12-24 | 2000-11-08 | Procédé de production d'un panneau de fibres léger à surface fermée |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP1110687B2 (fr) |
AT (1) | ATE313421T1 (fr) |
CY (1) | CY1104997T1 (fr) |
DE (2) | DE19963096C1 (fr) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102013103272A1 (de) * | 2013-04-02 | 2014-10-02 | Homatherm Gmbh | Verfahren zur Herstellung einer Faserplatte |
DE202017106335U1 (de) | 2017-10-19 | 2017-11-17 | Gce deutschland gmbh | Wellenfaserplatte im Nass- und Halbtrocken-Verfahren |
EP3272480A1 (fr) | 2016-07-21 | 2018-01-24 | GCE Deutschland GmbH | Procédé de fabrication d'un panneau de fibres |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10338007B4 (de) * | 2003-08-19 | 2005-12-29 | Glunz Ag | Verfahren zur Herstellung eines Dämmformkörpers aus leichtem Holzfaserdämmstoff und Dämmformkörper aus leichtem Holzfaserdämmstoff |
DE202006009318U1 (de) * | 2006-05-08 | 2007-09-20 | Dammers, Dirk | Platte, insbesondere Paneel zur Verkleidung von Wänden bzw. Decken oder als Bodenbelag |
DE102007019416A1 (de) * | 2006-07-19 | 2008-01-24 | Pfleiderer Holzwerkstoffe Gmbh & Co. Kg | Grundwerkstoff, dessen Herstellungsverfahren sowie Verwendung |
DE102007025801A1 (de) | 2007-06-02 | 2008-12-04 | Glunz Ag | Verfahren zur Herstellung eines leichten flexiblen Formkörpers auf der Basis von Lignocellulose haltigen Fasern |
EP2062709B1 (fr) | 2007-11-23 | 2012-06-13 | Glunz Ag | Plaques à base de fibres de bois encollées à l'aide d'un liant |
DE102010056491A1 (de) | 2009-12-23 | 2011-07-21 | Technische Universität Dresden, 01069 | Formkörper aus Pflanzenmaterial und Verfahren zu dessen Herstellung |
DE202014106187U1 (de) | 2014-12-19 | 2016-02-22 | Dieffenbacher GmbH Maschinen- und Anlagenbau | Dämm- und/oder Schallschutzplatte |
DE102014119242A1 (de) | 2014-12-19 | 2016-06-23 | Dieffenbacher GmbH Maschinen- und Anlagenbau | Dämm- und/oder Schallschutzplatte, deren Verwendung und ein Verfahren zur Herstellung von Dämm- und/oder Schallschutzplatten |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1184509A (fr) * | 1953-05-13 | 1959-07-22 | Procédé de fabrication de plaques de bois artificielles formées à partir de pctits morceaux de bois et de liants et plaques fabriquées par ce procédé | |
FR1103226A (fr) * | 1954-06-28 | 1955-10-31 | Rougier & Fils Sa | Panneaux en particules de bois agglomérés |
DE2538999C3 (de) * | 1975-09-02 | 1981-10-22 | Lignotock Verfahrenstechnik Gmbh, 1000 Berlin | Bindemittelkomponente für Polyurethan-Bindemittel |
US4175148A (en) * | 1976-11-05 | 1979-11-20 | Masonite Corporation | Product containing high density skins on a low density core and method of manufacturing same |
SE504637C2 (sv) * | 1995-07-27 | 1997-03-24 | Sunds Defibrator Ind Ab | Förfarande vid framställning av lignocellulosahaltiga skivor |
DE19604575A1 (de) * | 1996-02-08 | 1997-08-28 | Glunz Ag | Verfahren zur Herstellung von Span- oder Faserplatten |
DE19647240B4 (de) | 1996-11-15 | 2005-06-09 | Fritz Homann Gmbh & Co. Kg | Holzfaserplatte und Verfahren zu ihrer Herstellung |
-
1999
- 1999-12-24 DE DE19963096A patent/DE19963096C1/de not_active Expired - Fee Related
-
2000
- 2000-11-08 EP EP00124199A patent/EP1110687B2/fr not_active Expired - Lifetime
- 2000-11-08 DE DE50011903T patent/DE50011903D1/de not_active Expired - Lifetime
- 2000-11-08 AT AT00124199T patent/ATE313421T1/de active
-
2006
- 2006-03-20 CY CY20061100387T patent/CY1104997T1/el unknown
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102013103272A1 (de) * | 2013-04-02 | 2014-10-02 | Homatherm Gmbh | Verfahren zur Herstellung einer Faserplatte |
DE102013103272B4 (de) * | 2013-04-02 | 2016-09-15 | Homann Holzwerkstoffe GmbH | Verfahren zur Herstellung einer Sandwich-Faserplatte |
EP3272480A1 (fr) | 2016-07-21 | 2018-01-24 | GCE Deutschland GmbH | Procédé de fabrication d'un panneau de fibres |
DE202017106335U1 (de) | 2017-10-19 | 2017-11-17 | Gce deutschland gmbh | Wellenfaserplatte im Nass- und Halbtrocken-Verfahren |
Also Published As
Publication number | Publication date |
---|---|
DE50011903D1 (de) | 2006-01-26 |
DE19963096C1 (de) | 2001-05-03 |
EP1110687B1 (fr) | 2005-12-21 |
CY1104997T1 (el) | 2009-11-04 |
EP1110687A1 (fr) | 2001-06-27 |
ATE313421T1 (de) | 2006-01-15 |
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