EP0539924A1 - Procedure and apparatus for the production of transfer sheets for firing of images, characters, and decors on ceramic objects - Google Patents
Procedure and apparatus for the production of transfer sheets for firing of images, characters, and decors on ceramic objects Download PDFInfo
- Publication number
- EP0539924A1 EP0539924A1 EP92118362A EP92118362A EP0539924A1 EP 0539924 A1 EP0539924 A1 EP 0539924A1 EP 92118362 A EP92118362 A EP 92118362A EP 92118362 A EP92118362 A EP 92118362A EP 0539924 A1 EP0539924 A1 EP 0539924A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- printing
- transfer
- objects
- ceramic
- color pigments
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000919 ceramic Substances 0.000 title claims abstract description 27
- 238000012546 transfer Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 238000010304 firing Methods 0.000 title abstract description 8
- 239000000049 pigment Substances 0.000 claims abstract description 39
- 238000007639 printing Methods 0.000 claims abstract description 26
- 238000007646 gravure printing Methods 0.000 claims abstract description 16
- 238000009826 distribution Methods 0.000 claims abstract description 11
- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract 8
- 238000010023 transfer printing Methods 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000013405 beer Nutrition 0.000 claims description 6
- 238000005034 decoration Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000007650 screen-printing Methods 0.000 claims description 6
- 238000002485 combustion reaction Methods 0.000 claims description 4
- JLBXCKSMESLGTJ-UHFFFAOYSA-N 1-ethoxypropan-1-ol Chemical compound CCOC(O)CC JLBXCKSMESLGTJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000011877 solvent mixture Substances 0.000 claims description 3
- IOPYVZVNUXHZCP-UHFFFAOYSA-N 2-(3-ethyloctan-3-yloxycarbonyl)benzoic acid Chemical compound CCCCCC(CC)(CC)OC(=O)C1=CC=CC=C1C(O)=O IOPYVZVNUXHZCP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000020 Nitrocellulose Substances 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- MJEMIOXXNCZZFK-UHFFFAOYSA-N ethylone Chemical compound CCNC(C)C(=O)C1=CC=C2OCOC2=C1 MJEMIOXXNCZZFK-UHFFFAOYSA-N 0.000 claims description 2
- 230000002401 inhibitory effect Effects 0.000 claims description 2
- 229920001220 nitrocellulos Polymers 0.000 claims description 2
- -1 polyethylene Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000009472 formulation Methods 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 238000004040 coloring Methods 0.000 abstract description 6
- 239000002152 aqueous-organic solution Substances 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 6
- 239000003086 colorant Substances 0.000 description 5
- 238000013461 design Methods 0.000 description 3
- 235000011837 pasties Nutrition 0.000 description 3
- 239000002966 varnish Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 238000007645 offset printing Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010017 direct printing Methods 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M3/00—Printing processes to produce particular kinds of printed work, e.g. patterns
- B41M3/12—Transfer pictures or the like, e.g. decalcomanias
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/26—Printing on other surfaces than ordinary paper
- B41M1/34—Printing on other surfaces than ordinary paper on glass or ceramic surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B44—DECORATIVE ARTS
- B44C—PRODUCING DECORATIVE EFFECTS; MOSAICS; TARSIA WORK; PAPERHANGING
- B44C1/00—Processes, not specifically provided for elsewhere, for producing decorative surface effects
- B44C1/16—Processes, not specifically provided for elsewhere, for producing decorative surface effects for applying transfer pictures or the like
- B44C1/165—Processes, not specifically provided for elsewhere, for producing decorative surface effects for applying transfer pictures or the like for decalcomanias; sheet material therefor
- B44C1/175—Transfer using solvent
- B44C1/1756—Decalcomanias applied under heat and pressure, e.g. provided with a heat activable adhesive
Definitions
- the invention relates to a method and a device for the production of transfer printing papers for the burning of images, writing and decorations on ceramic objects to be burned, such as crockery parts, tiles or on objects that retain their shape at a high heating temperature, such as beer bottles, with the image and / or lettering and / or decorations provided transfer printing papers are attached to the objects on the color pigment side and are burned or heated together with them.
- Ceramic color pigments are used for the image or decor of ceramic objects of the type mentioned, which differ significantly from normal color pigments used in other printing processes, since these ceramic color pigments have to be fired together with the shaped ceramic blanks.
- ceramic color pigments cannot be applied directly to the objects, but this is done using so-called transfer papers, which, as far as is known, have so far only been produced in offset printing or screen printing for this special work area to at least approximately achieve an identity of the individual prints with one another.
- transfer papers represent "decals” to a certain extent, which are fixed in a suitable manner on the objects to be decorated. However, these "decals” are not “peeled off” in the conventional sense, but their backing papers simply burn away at the relatively high firing temperatures (800 to 1,200 ° C.), but at the same time the color pigments burn up.
- the transfer paper is placed on the screen printing device, a screen is pressed onto the sheet and then is passed through the screen, i.e. whose free parts of the image are squeezed through the pasty paint by means of a squeegee and thus applied to the transfer paper, which then has to be dried for several hours.
- This application is rather imprecise, so that a reject of up to 60% often arises, since here again, color by color must be applied. This results in even longer production times, and the entire screen printing process is inaccurate, since the screen, a mechanical part and the coloring depend on the individual handling and are therefore not controllable in standards.
- the invention has for its object to provide a method and a device for its implementation for the production of transfer printing papers, specifically for the present special area, which neither a variety of Printing processes still require the use of varnish and powder orders and long drying times, which should be feasible in a normative manner and which leads to optimal and always identical firing results of the image or decor design on the ceramic objects.
- DE-A-24 08 899 and DE-A-28 28 320 the use of the rotogravure process for the production of transfer papers has already been mentioned, but DE-A-24 08 899 is exclusively about it in the usual way To design and treat disperse dyes produced in this way and which are unfavorable for gravure printing in such a way that they obtain the flowability required for gravure printing, which should also be retained over long periods of time.
- DE-A-28 28 320 relates to a gravure printing machine for printing transfer papers, but it is not about printing the transfer papers per se, but rather to provide these transfer papers with a so-called separating layer on the back, which acts as a diffusion barrier should work for the printed colors, which is absolutely irrelevant for the present case.
- the color pigments must be present in the solvent in a relatively high proportion, that they must be kept in a homogeneous distribution in the solvent mixture, and that the cell depth of the screen printing form must be comparatively deep (normal 30 ⁇ ; here at least 50 - 100 ⁇ ) and that finally a relatively high proportion of an anti-combustion additive must be contained in the solvent mixture.
- beer bottles as has been shown, can now also be provided in this way instead of the usual labeling with corresponding images, text and decorations, which is only required once , because the color pigment firing lasts at least as long as it corresponds to the average life span of a beer bottle.
- previous attempts to replace the labeling with other options have failed on their own because in this connection the initially suitable color application methods did not allow the production of fine-line codes, as are common today.
- the device or the gravure printing machine for carrying out the method consists of an intaglio cylinder 1 with a doctor blade 2 and an associated printing cylinder 3 and an ink reservoir 4 from which the ink is transferred directly or indirectly to the forme cylinder 1 by means of transfer cylinders 5 (see FIG. 2) is, and from conveying elements for feeding the Bedurckmaterials between the form and pressure cylinders 1, 3rd
- a circulation circuit 7 with a circulation pump 8 on the storage container, the circulation pump 8 being expediently arranged on the return connection 11 opening at the top of the storage container.
- the ink supply line and an overflow required to maintain the immersion level for the gravure cylinder 1 are not shown on the reservoir 4. 2, which is used in particular for short runs, applies practically the same, ie the reservoir 4 there is also equipped with a homogenizer 6 as described above.
- a homogenizer 6 as described above.
Landscapes
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Printing Methods (AREA)
- Decoration By Transfer Pictures (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren und eine Vorrichtung zur Herstellung von Transferdruckpapieren für das Aufbrennen von Bild-, Schrift- und Dekordarstellungen auf zu brennende Keramikgegenstände, wie Geschirrteile, Fliesen oder auf bei hoher Erhitzungstemperatur formbeständig bleibende Gegenstände, wie Bierflaschen, wobei die mit der Bild- und/oder Schrift- und/oder Dekordarstellung versehenen Transferdruckpapiere an den Gegenständen farbpigmentseitig angeheftet und mit diesen zusammen gebrannt bzw. erhitzt werden.The invention relates to a method and a device for the production of transfer printing papers for the burning of images, writing and decorations on ceramic objects to be burned, such as crockery parts, tiles or on objects that retain their shape at a high heating temperature, such as beer bottles, with the image and / or lettering and / or decorations provided transfer printing papers are attached to the objects on the color pigment side and are burned or heated together with them.
Für die Bild- oder Dekorausstattung von Keramikgegenständen der genannten Art werden Keramikfarbpigmente benutzt, die sich wesentlich von normalen, bei sonstigen Druckverfahren zur Anwendung kommenden Farbpigmenten unterscheiden, da diese Keramikfarbpigmente zusammen mit den ausgeformten Keramikrohlingen gebrannt werden müssen. Insofern können, sieht man von deren individuellem Direktfarbauftrag per Hand bzw. per Pinsel ab, Keramikfarbpigmente auch nicht direkt auf die Gegenstände aufgebracht werden, sondern dies geschieht mittels sogenannter Transferpapieren, die, soweit bekannt, für diesen speziellen Arbeitsbereich bisher nur im Offsetdruck oder Siebdruck hergestellt werden , um wenigstens in etwa eine Identität der Einzeldrucke untereinander zu erreichen. Diese Transferpapiere stellen gewissermaßen "Abziehbilder" dar, die auf den zu dekorierenden Gegenständen in geeigneter Weise fixiert werden. Diese "Abziehbilder" werden jedoch nicht im herkömmlichen Sinne "abgezogen", sondern deren Trägerpapiere brennen bei den relativ hohen Brenntemperaturen (800 bis 1.200°C) einfach weg, wobei jedoch gleichzeitig die Farbpigmente aufbrennen.Ceramic color pigments are used for the image or decor of ceramic objects of the type mentioned, which differ significantly from normal color pigments used in other printing processes, since these ceramic color pigments have to be fired together with the shaped ceramic blanks. In this respect, apart from their individual direct color application by hand or with a brush, ceramic color pigments cannot be applied directly to the objects, but this is done using so-called transfer papers, which, as far as is known, have so far only been produced in offset printing or screen printing for this special work area to at least approximately achieve an identity of the individual prints with one another. These transfer papers represent "decals" to a certain extent, which are fixed in a suitable manner on the objects to be decorated. However, these "decals" are not "peeled off" in the conventional sense, but their backing papers simply burn away at the relatively high firing temperatures (800 to 1,200 ° C.), but at the same time the color pigments burn up.
Beim Offsetdruck solcher Transferdruckpapiere kann jedoch für deren Herstellung auch kein Direktdruck mit den angeteigten Farbpigmenten erfolgen, sondern gedruckt wird zunächst ein klebriger Firnis, der anschließend von einer Pudermaschine mit den Farbpigmenten einer Farbe bepudert wird, wobei die Keramikfarbpigmente am aufgedruckten Firnis kleben bleiben und die nicht haftenden Pigmente entfernt werden. Bei diesem Verfahren sind je nach Dekorgestaltung bis zu vierundzwanzig Durchgänge für jede Einzelfarbe erforderlich, um die einzelnen Farben überhaupt aufbringen zu können. Dies bedeutet sehr lange Herstellungszeiten, sehr hohe Kosten und vor allen Dingen eine Ungenauigkeit, wie sie bei den heutigen Anforderungen nicht mehr akzeptabel ist aber nach wie vor hingenommen werden muss. Etwa notwendige Nachbestellungen für bspw. zu Bruch gegangene Keramikgegenstände weichen dann, da aus einem anderen Fertigungsvorgang stammend, mitunter beträchtlich in ihrem Erscheinungsbild von den Originalgegenständen ab.In offset printing of such transfer printing papers, however, no direct printing with the pasted color pigments can take place for their production, but instead a sticky varnish is printed, which is then powdered with the color pigments of one color by a powder machine, the ceramic color pigments sticking to the printed varnish and that non-stick pigments are removed. Depending on the decor design, this process requires up to twenty-four passes for each individual color in order to be able to apply the individual colors at all. This means very long manufacturing times, very high costs and, above all, an inaccuracy that is no longer acceptable with today's requirements but still has to be accepted. Any necessary re-orders for ceramic objects that have broken, for example, then, because they originate from a different manufacturing process, sometimes differ considerably in their appearance from the original objects.
Bei der zweiten, bisher ebenfalls nur für diesen speziellen Arbeitsbereich praktizierten Art zur Hestellung der Transferdruckpapiere, nämlich dem Siebdruck, wird das Transferpapier auf der Siebdruckvorrichtung angelegt, ein Sieb auf den Bogen aufgepreßt und dann wird durch das Sieb, d.h. dessen freie Bildteile mittels eines Rakels die pastös angesetzte Farbe durchgequetscht und damit auf das Transferpapier aufgebracht, das dann mehrere Stunden getrocknet werden muß. Diese Aufbringung ist ziemlich ungenau, so daß häufig ein Ausschuß von bis zu 60 % entsteht, da auch hier wiederum Farbe für Farbe aufgetragen werden muß. Hierbei ergeben sich noch längere Herstellungszeiten, und das ganze Siebdruckverfahren ist ungenau, da das Sieb ein mechanisches Teil und die Farbgebung von der individuellen Handhabung abhängig und damit auch nicht in Normen steuerbar ist. Die Nachteile entsprechen praktisch denen des vorerwähnten Offsetverfahrens, und von einem nach DIN-Normen durchführbaren Produktionsprozeß sind diese bisher praktizierten Methoden weit entfernt. Trotz der in der Regel hohen Stückzahlanforderungen hat man sich bislang damit jedoch abfinden müssen und abgefunden, da keine anderen Methoden zur Verfügung standen.In the second method of producing the transfer printing papers, namely screen printing, which has also previously only been used for this special working area, the transfer paper is placed on the screen printing device, a screen is pressed onto the sheet and then is passed through the screen, i.e. whose free parts of the image are squeezed through the pasty paint by means of a squeegee and thus applied to the transfer paper, which then has to be dried for several hours. This application is rather imprecise, so that a reject of up to 60% often arises, since here again, color by color must be applied. This results in even longer production times, and the entire screen printing process is inaccurate, since the screen, a mechanical part and the coloring depend on the individual handling and are therefore not controllable in standards. The disadvantages correspond practically to those of the above-mentioned offset process, and these previously practiced methods are far removed from a production process which can be carried out according to DIN standards. Despite the generally high demands on the number of pieces, it has so far been accepted and resigned, since no other methods were available.
Der Erfindung liegt die Aufgabe zugrunde, für die Herstellung von Transferdruckpapieren, und zwar für den hier vorliegenden speziellen Bereich, ein Verfahren und eine Vorrichtung zu seiner Durchführung zu schaffen, das weder einer Vielzahl von Druckvorgängen noch der Verwendung von Firnis- und Puderaufträgen und langer Trocknungszeiten bedarf, das normativ durchführbar sein soll und das zu optimalen und immer identischen Aufbrennergebnissen der Bild- oder Dekorgestaltung an den keramischen Gegenständen führt.The invention has for its object to provide a method and a device for its implementation for the production of transfer printing papers, specifically for the present special area, which neither a variety of Printing processes still require the use of varnish and powder orders and long drying times, which should be feasible in a normative manner and which leads to optimal and always identical firing results of the image or decor design on the ceramic objects.
Diese Aufgabe ist mit einem Verfahren der eingangs genannten Art nach der Erfindung durch die im Kennzeichen des Anspruchs 1 angeführten Merkmale gelöst.This object is achieved with a method of the type mentioned at the outset according to the invention by the features stated in the characterizing part of
Mit der Verwendung einer wässrigen, organischen Lösung, die für den vorliegenden Fall einen verbrennungsbremsenden Zusatz enthalten muß und in der die Farbpigmente homogen verteilt und auch während des Druckvorganges in homogener Verteilung gehalten werden müssen, was wesentlich ist, ist die Voraussetzung geschaffen, für den vorliegenden Zweck das an sich bekannte Tiefdruckverfahren anwenden zu können, mit dem lediglich und in bekannter Weise die drei Grundfarben und ggf. auch Schwarz und Gold zu drucken sind. An herkömmlichen Tiefdruckmaschinen, egal ob Bogendruckmaschine oder kontinuierlich arbeitende Tiefdruckrotationsmaschine, sind Änderungen nur insofern vorzunehmen, als am Farbvorratsbehälter ein Homogenisator vorgesehen werden muß, der dafür sorgt, daß die Farbpigmente im Lösungsansatz während des Druckens immer in homogener Verteilung enthalten sind und auch mit dieser homogenen Verteilung in die druckenden Näpfchen des Formzylinders gelangen, der entweder direkt in den Lösungsansatz eintaucht oder seine ständige Farbzufuhr durch einen Übertragungszylinder erhält, der seinerseits in den Lösungsansatz eintaucht. Zur Erklärung dafür, daß bisher für den genannten Zweck offenbar noch nie das wesentlich genauere und rationellere Tiefdruckverfahren angewendet wurde, kann nur vermutet werden, daß man wegen der Entmischungstendenz schwerer Keramikfarbpigmente meinte, diese nur in teigig, pastöser Form verarbeiten zu können und damit das Tiefdruckverfahren außer Betracht zu bleiben hatte. Außerdem dürften Hinderungsgrund und Denkhemmung gewesen sein, die nicht ohne weiteres zusammenzubringenden Gesichtspunkte einerseits die für den Tiefdruck normalerweise notwendige, flüssigere Konsistenz der Keramikfarben, um sie dem Tiefdruck überhaupt zugänglich zu machen und andererseits der erforderliche, im Vergleich zu normalen, im Tiefdruck zu verarbeitenden Farben wesentlich stärkere Farbauftrag, um trotz des Brennvorganges überhaupt eine befriedigende Bild- bzw. Dekorwiedergabe zu erreichen.With the use of an aqueous, organic solution, which for the present case must contain a combustion-inhibiting additive and in which the color pigments must be distributed homogeneously and must also be kept in a homogeneous distribution during the printing process, which is essential, the prerequisite has been created for the present Purpose of being able to use the gravure printing method known per se, with which the three primary colors and possibly also black and gold can only be printed in a known manner. Changes to conventional rotogravure printing machines, regardless of whether they are sheet-fed printing presses or continuous rotogravure printing presses, should only be made to the extent that a homogenizer must be provided on the ink reservoir, which ensures that the color pigments in the solution are always contained in a homogeneous distribution during printing and also with this homogenous distribution Distribution get into the printing wells of the forme cylinder, which either dips directly into the solution or receives its constant ink supply through a transfer cylinder, which in turn dips into the solution. To explain why the much more precise and rational gravure printing process has apparently never been used for the stated purpose, it can only be assumed that due to the tendency towards segregation of heavy ceramic color pigments, it was thought that they could only be processed in pasty, pasty form and thus the gravure printing process had to be disregarded. In addition, the reason for hindrance and inhibition of thinking may have been the points of view that cannot easily be brought together on the one hand, the more fluid consistency normally required for gravure printing the ceramic inks in order to make them accessible to rotogravure at all, and on the other hand the required, in comparison to normal, to be processed in rotogravure colors much stronger application of paint in order to achieve a satisfactory image or decor reproduction despite the firing process.
In der DE-A-24 08 899 und der DE-A-28 28 320 ist zwar die Anwendung des Tiefdruckverfahrens für die Herstellung von Transferpapieren schon angesprochen, bei der DE-A-24 08 899 handelt es sich aber ausschließlich darum, in üblicher Weise hergestellte und für den Tiefdruck ungünstige Viskositätseigenschaften aufweisende Dispersionsfarbstoffe so zu gestalten und zu behandeln, daß diese die für den Tiefdruck erforderliche Fließfähigkeit erhalten, die dabei auch über längere Zeiträume erhalten bleiben soll. Die DE-A-28 28 320 bezieht sich demgegenüber auf eine Tiefdruckmaschine zum Bedrucken von Transferpapieren, wobei es jedoch nicht um das Bedrucken der Transferpapiere an sich geht, sondern darum, diese Transferpapiere auf der Rückseite mit einer sogenannten Trennschicht zu versehen, die als Diffusionssperre für die aufgedruckten Farben wirken soll, was für den vorliegenden Fall absolut irrelevant ist.In DE-A-24 08 899 and DE-A-28 28 320 the use of the rotogravure process for the production of transfer papers has already been mentioned, but DE-A-24 08 899 is exclusively about it in the usual way To design and treat disperse dyes produced in this way and which are unfavorable for gravure printing in such a way that they obtain the flowability required for gravure printing, which should also be retained over long periods of time. DE-A-28 28 320, on the other hand, relates to a gravure printing machine for printing transfer papers, but it is not about printing the transfer papers per se, but rather to provide these transfer papers with a so-called separating layer on the back, which acts as a diffusion barrier should work for the printed colors, which is absolutely irrelevant for the present case.
Für die erfindungsgemäße Lösung, die sich also nicht allein auf die Anweisung beschränkt, nunmehr die Keramikfarben einfach per Tiefdruck auf das Transferpapier zu übertragen, sondern die in Kombination ganz wesentliche erfinderische Zusatzmaßnahmen verlangt, nämlich die Verwendung verbrennungshemmender Zusätze, extreme Näpfchentiefen und die Aufrechterhaltung der Homogenität des entgegen bisheriger Praxis bei der Keramikfarbübertragung ausreichend für den Tiefdruck geeigneter flüssiger Konsistenz angesetzten Farbansatzes im Farbvorratsbehälter, hat sich für die wässrige, organische Lösung ein Lösungsansatz als Trägersubstanz für die Farbpigmente gebildet aus
- a) Ethoxypropanol
- b) Ethanol
- c) Di-ethylhexylphtalat
- d) Nitrozellulose
- e) Ethylacetat und einer
- f) Polyäthylenwachsdispersion
- a) 80 - 120
- b) 490 - 520
- c) 50 - 70
- d) 190 - 210
- e) 90 - 110
- f) 25 - 45.
- a) ethoxypropanol
- b) ethanol
- c) Di-ethylhexyl phthalate
- d) nitrocellulose
- e) ethyl acetate and one
- f) polyethylene wax dispersion
- a) 80-120
- b) 490 - 520
- c) 50-70
- d) 190-210
- e) 90-110
- f) 25-45.
Es hat sich überraschenderweise gezeigt daß sich damit im Tiefdruck trotz der Verwendung schwerer, zur Entmischung neigender Keramikfarbpigmente einwandfrei bedruckte Transferpapiere und damit ausgezeichnete und identisch reproduzierbare Brennergebnisse für die mit Bildern oder Dekor zu versehenden Keramikgegenstände erzielen lassen. Die verwendeten Keramikfarbpigmente hatten dabei eine Korngröße von < 5µ und waren im Lösungsansatz mit 40 - 65 Gew.-% während des Druckvorganges homogen verteilt. Bezüglich der in das Lösungsmittel einzubringenden Pigmentmenge ist letztlich maßgebend, daß der gesamte verarbeitbare Lösunsmittel-Pigmentansatz gerade noch ausreichend wässrig und damit tiefdruckbar sein muß. Die angegebene Bereichsbreite der Gewichts-% hat ihren Grund darin, ob bspw. Hart- oder Weichporzellan dekoriert werden soll und um welche Farbe der Pigmente es sich handelt.Surprisingly, it has been found that in gravure printing, despite the use of heavy ceramic color pigments that tend to separate, perfectly printed transfer papers and thus excellent and identically reproducible firing results can be achieved for the ceramic objects to be provided with images or decor. The ceramic color pigments used had a grain size of <5µ and were homogeneously distributed in the solution with 40-65% by weight during the printing process. With regard to the amount of pigment to be introduced into the solvent, it is ultimately decisive that the entire processable solvent-pigment batch just has to be sufficiently watery and thus capable of being deeply printed. The range width of the% by weight is based on whether, for example, hard or soft porcelain is to be decorated and which color of the pigments it is.
Zusammenfassend ist also für die Anwendbarkeit des an sich bekannten Tiefdruckverfahrens insgesamt wesentlich, daß die Farbpigmente mit einem relativ hohen Anteil im Lösungsmittel enthalten sein müssen, daß diese im Lösungsmittelansatz in homogener Verteilung gehalten werden müssen, daß die Näpfchentiefe der Rasterdruckform vergleichsweise tief sein muß (normal 30µ; hier mindestens 50 - 100µ) und daß schließlich im Lösungsmittelansatz ein relativ hoher Anteil eines verbrennungsbremsenden Zusatzes enthalten sein muß.In summary, it is essential for the applicability of the gravure printing process, which is known per se, that the color pigments must be present in the solvent in a relatively high proportion, that they must be kept in a homogeneous distribution in the solvent mixture, and that the cell depth of the screen printing form must be comparatively deep (normal 30µ; here at least 50 - 100µ) and that finally a relatively high proportion of an anti-combustion additive must be contained in the solvent mixture.
Was den "verbrennungsbremsenden" Zusatz im Lösungsmittel betrifft, so ist dieser besonders wichtig, denn bei Vorversuchen hat sich gezeigt, daß bei nicht vorhandenem oder in zu geringer Menge zugesetztem Zusatz dieser Art - dafür haben sich Wachsdispersionszusätze als geeignet erwiesen - der Lösungsmittelansatz gewissermaßen explosionsartig unter Mitnahme eines großen Teiles der Farbpigmente verpufft und damit für den Farbauftrag verlorengehen.As far as the "anti-combustion" additive in the solvent is concerned, this is particularly important, because it has been shown in preliminary tests that if this type of additive is not present or is added in too small amount - wax dispersion additives have proven to be suitable - the solvent mix is explosive to a certain extent Carrying away a large part of the color pigments fizzles out and is therefore lost for the color application.
Was die vorerwähnte zusätzliche Zweckbestimmung der Transferpapiere für auf bei hoher Erhitzungstemperatur formbeständig bleibende Gegenstände, insbesondere Bierflaschen betrifft, so ist damit eine besondere Problematik angesprochen. Bekanntlich werden Bierflaschen etikettiert. Nach Rückgabe der Flaschen müssen die Altetiketten mit chemischen Behandlungsmitteln (Säurebad) entfernt werden, wobei insgesamt gesehen, enorme Mengen von mit dem Behandlungsmitteln behaftete Etikettenreste anfallen, die in Rücksicht auf Umweltbealstung einer Sonderentsorgung bedürfen, welches Problem bis jetzt überhaupt noch nicht befriedigend gelöst werden konnt. In Rücksicht auf die durch die erfindungsgemäße Lösung möglich gewordene kostengünstige Herstellung von Transferpapieren können nunmehr auch Bierflaschen, wie sich gezeigt hat, ebenfalls auf diese Weise statt der bisher üblichen Etikettierung mit entsprechenden Bild-, Schrift- und Dekordarstellungen versehen werden, was nur einmalig erforderlich ist, da der Farbpigmentaufbrand mindestens so lange haltbar ist, wie es der durchschnittlich angesetzten Lebensdauer einer Bierflasche entspricht. Soweit bekannt, sind bisherige Versuche, die Etikettierungen durch andere Möglichkeiten zu ersetzen, allein schon daran gescheitert, daß es in diesem Zusammenhang die zunächst geeignet erscheinende Farbauftragsmethoden nicht zuließen, feinstrichige Codierungen, wie sie heute üblich sind, mit herzustellen.With regard to the aforementioned additional intended use of the transfer papers for objects that remain dimensionally stable at high heating temperatures, in particular beer bottles, this addresses a particular problem. As is well known, beer bottles are labeled. After returning the bottles, the old labels with chemical treatment agents (acid bath) have to be removed, whereby overall there are enormous amounts of label residues with the treatment agents that require special disposal in view of environmental pollution, which problem has not yet been satisfactorily solved . In view of the cost-effective production of transfer papers made possible by the solution according to the invention, beer bottles, as has been shown, can now also be provided in this way instead of the usual labeling with corresponding images, text and decorations, which is only required once , because the color pigment firing lasts at least as long as it corresponds to the average life span of a beer bottle. As far as is known, previous attempts to replace the labeling with other options have failed on their own because in this connection the initially suitable color application methods did not allow the production of fine-line codes, as are common today.
Obgleich die Vorrichtun bzw. Tiefdruckmaschine, wie erwähnt, zur Durchführung des Verfahrens nur geringfügiger Abänderungen bedarf, die an sich ohne weiteres vorstellbar sind, sei dies nachfolgend anhand der zeichnerischen Darstellung zweier Ausführunsbeispiele näher erläutert.Although, as mentioned, the device or rotogravure printing press requires only minor modifications to carry out the method, which are in themselves readily conceivable, this is the case explained in more detail below with reference to the drawing of two exemplary embodiments.
Es zeigt schematisch
- Fig. 1
- das Farbgebungssystem für den Druck einer Farbe an einer kontinuierlich arbeitenden, ansonsten aber nicht dargestellten Rotationstiefdruckmaschine und
- Fig. 2
- das Prinzip einer Bogendruckmaschine.
- Fig. 1
- the coloring system for printing a color on a continuously working, but not shown rotogravure printing machine and
- Fig. 2
- the principle of a sheet printing machine.
Die Vorrichtung bzw. die Tiefdruckmaschine zur Durchführung des Verfahrens besteht aus einem Tiefdruckzylinder 1 mit Rakel 2 und zugeordnetem Druckzylinder 3 und aus einem Farbvorratsbehälter 4, aus dem die Farbe direkt oder indirekt mittels Übertragungszlinder 5 (s. Fig. 2) auf den Formzylinder 1 übertragen wird, und aus Förderelementen zur Zuführung des Bedurckmaterials zwischen die Form- und Druckzylinder 1, 3.The device or the gravure printing machine for carrying out the method consists of an
Um nun die in der wässrigen, organischen Lösung angesetzten Keramikfarbpigmente im Tiefdruckverfahren auf das Transferdruckpapier 10, 10' per Druck übertragen und die Farbpigmente vor ihrer Übernahme auf den Tiefdruckformzylinder 1 in homogener Verteilung im Lösungsansatz halten zu können, ist im Farbvorratsbehälter 4 ein die homogene Verteilung der Farbpigmente in der wässrigen, organischen Lösung aufrechtzuerhaltender Homogenisator 6 angeordnet, wie dies in Fig. 1 dargestellt ist, in der bspw. zwei schnellaufende Schneckenrührer 6' in den Vorratsbehälter 4 einragen. Stattdessen oder ergänzend, wie dargestellt, ist es aber auch möglich, am Vorratsbehälter einen Umlaufkreis 7 mit einer Umwälzpumpe 8 vorzusehen, wobei die Umwälzpumpe 8 zweckmäßig am oben am Vorratsbehälter einmündenden Rücklaufanschluß 11 angeordnet ist. Nicht dargestellt ist am Vorratsbehälter 4 die notwendige Farbzufuhrleitung und ein Überlauf, um das Tauchniveau für den Tiefdruckzylinder 1 aufrechtzuerhalten. Für die Bogentiefdruckmaschine gemäß Fig. 2, die insbesondere für kleinere Auflagen verwendet wird, gilt praktisch das gleiche, d.h. der dortige Vorratsbehälter 4 ist ebenfalls mit einem Homogenisator 6 wie vorbeschrieben ausgestattet. Nur der Vollständigkeit halber sei darauf hingewiesen, daß beim Drei- oder Vierfarbdruck von Transferdruckpapier eine entsprechende Anzahl von Druckwerken bzw. Drucksystemen, wie in Fig. 1, 2 dargestellt, hinereinander angeordnet werden müssen.In order to transfer the ceramic color pigments used in the aqueous, organic solution to the
Um den Benutzern des Verfahrens nicht die richtige anteilsmäßige Zusammensetzung für den zu druckenden Farbansatz zu überlassen und auch insoweit eine normative Vorgabe zu machen, ist es vorteilhaft, und zwar trotz erwartbarer Entmischung von Lösungsmittel und Keramikfarbpigmenten bzw. deren Sedimentation, den Gesamtansatz aus Lösungsmittel und Pigmenten in einem Transport- und Lagerbehälter unterzubringen und insoweit verarbeitungsfertig zur Verfügung zu stellen, wobei sich natürlich vor dem Ausgießen in den Vorratsbehälter 4 eine gute Durchmischung empfiehlt. Die Anheftung der fertig gedruckten Transferdruckpapiere an den zu dekorierenden und zu brennenden Gegenständen erfolgt im übrigen einfach durch Anfeuchten und Anpressen vor dem Brennen.In order not to leave the correct proportionate composition for the color batch to be printed to the users of the process and also to make a normative specification in this respect, it is advantageous, despite expected separation of solvents and ceramic color pigments or their sedimentation, the total batch of solvents and pigments to be accommodated in a transport and storage container and, in this respect, to be made available ready for processing, a thorough mixing of which is of course recommended before pouring into the
Claims (10)
dadurch gekennzeichnet,
daß die Keramikfarbpigmente in einer wässrigen, organischen, einen verbrennungsbremsenden Zusatz enthaltenden Lösung angesetzt und im Tiefdruckverfahren unter Verwendung von Druckformen mit einer Näpfchentiefe von mindestens 50 - 100µ auf das Transferdruckpapier übertragen und die Farbpigmente vor ihrer Übernahme auf den Tiefdruckzylinder in homogener Verteilung im Lösungsansatz gehalten werden.Process for the production of transfer printing papers for the burning of images, writing and decorations on ceramic objects to be burned, such as crockery parts, tiles or on objects that retain their shape at a high heating temperature, such as beer bottles, the ones with the image and / or writing and / transfer decorations provided with decorations are attached to the objects on the color pigment side and burned or heated together with them,
characterized,
that the ceramic color pigments are prepared in an aqueous, organic solution containing a combustion-inhibiting additive and transferred to the transfer printing paper in the gravure printing process using printing formes with a well depth of at least 50-100 μm, and the color pigments are kept in a homogeneous distribution in the solution mixture before they are transferred to the gravure printing cylinder .
dadurch gekennzeichnet,
daß für die wässrige, organische Lösung ein Ansatz verwendet wird, der gebildet ist aus
characterized,
that an approach is used for the aqueous, organic solution, which is formed from
dadurch gekennzeichnet,
daß die Lösungskomponenten in der Lösung mit folgenden Anteilen verwendet werden:
characterized,
that the solution components are used in the solution in the following proportions:
dadurch gekennzeichnet,
daß die Keramikfarbpigmente mit einer Korngröße < 10µ, vorzugsweise < 5µ der wässrigen Lösung mit 40 - 65 Gew.-% zugesetzt werden.Method according to claim 2 or 3,
characterized,
that the ceramic color pigments with a grain size <10µ, preferably <5µ are added to the aqueous solution with 40-65% by weight.
dadurch gekennzeichnet,
daß im Farbvorratsbehälter (4) ein die homogene Verteilung der Farbpigmente in der wässrigen, organischen Lösung aufrechterhaltender Homogenisator (6) angeordnet ist und daß die Rasterdruckform eine Näpfchentiefe von mindestens 50 - 100µ aufweist.Apparatus for carrying out the method according to claim 1, consisting of an intaglio printing cylinder (1) equipped with the raster printing forms with doctor blade (2) and associated printing cylinder (3) and of an ink reservoir (4) from which the ink is transferred directly or indirectly by means of transfer cylinders (5 ) is transferred to the forme cylinder (1) and from conveying elements for feeding the printing material between the forme and impression cylinders (1, 3),
characterized,
that a homogenizer (6) which maintains the homogeneous distribution of the color pigments in the aqueous, organic solution is arranged in the ink reservoir (4) and that the screen printing form has a well depth of at least 50-100μ.
dadurch gekennzeichnet,
daß der Homogenisator (6) als Rührer ausgebildet ist.Device according to claim 5,
characterized,
that the homogenizer (6) is designed as a stirrer.
dadurch gekennzeichnet,
daß der Homogenisator (6) am Vorratsbehälter (4) in Form eines Umwälzkreises (7) mit Umwälzpumpe (8) ausgebildet ist.Apparatus according to claim 5 or 6,
characterized,
that the homogenizer (6) on the reservoir (4) is designed in the form of a circulation circuit (7) with a circulation pump (8).
dadurch gekennzeichnet,
daß die Umwälzpumpe (8) am oben am Vorratsbehälter (4) angeordneten Rücklaufanschluß (11) angeordnet ist.Device according to claim 7,
characterized,
that the circulation pump (8) is arranged on the return port (11) arranged at the top of the storage container (4).
dadurch gekennzeichnet,
daß die Keramikfarbpigmente zusammen mit dem Lösungsmittelansatz mit einer qualitativen und quantitativen Zusammensetzung gemäß der Ansprüche 2 bis 4 in einem Transport- und Lagerbehälter enthalten sind.Ceramic color pigment formulation for carrying out the method according to claim 1,
characterized,
that the ceramic color pigments are contained in a transport and storage container together with the solvent mixture with a qualitative and quantitative composition according to claims 2 to 4.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4135620 | 1991-10-29 | ||
| DE4135620 | 1991-10-29 | ||
| DE4203162A DE4203162A1 (en) | 1991-10-29 | 1992-02-05 | METHOD AND DEVICE FOR PRODUCING TRANSFER PRINTING PAPERS |
| DE4203162 | 1992-02-05 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0539924A1 true EP0539924A1 (en) | 1993-05-05 |
| EP0539924B1 EP0539924B1 (en) | 1996-03-20 |
Family
ID=25908617
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP92118362A Expired - Lifetime EP0539924B1 (en) | 1991-10-29 | 1992-10-28 | Procedure and apparatus for the production of transfer sheets for firing of images, characters, and decors on ceramic objects |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP0539924B1 (en) |
| AT (1) | ATE135637T1 (en) |
| DE (2) | DE4203162A1 (en) |
| DK (1) | DK0539924T3 (en) |
| ES (1) | ES2086045T3 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995015266A1 (en) * | 1993-12-02 | 1995-06-08 | Cookson Matthey Print Limited | Method of producing transfer sheets |
| WO1996001745A1 (en) * | 1994-07-12 | 1996-01-25 | F. Xaver Leipold Gmbh & Co. Kg | Process for making ceramic transfer images by offset printing |
| WO1998055327A1 (en) * | 1997-06-04 | 1998-12-10 | University Of The West Of England, Bristol | Printing onto a heat-resistant base |
| GB2340791A (en) * | 1997-06-04 | 2000-03-01 | Univ Bristol | Printing onto a heat-resistant base |
| EP1369263A1 (en) * | 2002-05-31 | 2003-12-10 | Tecno-Europa S.r.l. | Method and processing unit for producing decorated sheets for decorating ceramic articles |
| CN107336535A (en) * | 2017-07-24 | 2017-11-10 | 青州新华包装制品有限公司 | A kind of printing process of laser packaging product and the all-in-one using this method |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4414270C2 (en) | 1994-04-23 | 1998-12-03 | Manfred Neuberger | Process for the production of transfer printing papers |
| DE19513888A1 (en) * | 1995-04-19 | 1996-10-24 | Focke & Co | Method and device for applying markings, in particular color markings, to film webs |
| DE19605975A1 (en) * | 1996-02-17 | 1997-08-21 | Heraeus Gmbh W C | Printing medium for ceramic color preparations |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR343180A (en) * | 1904-05-16 | 1904-09-27 | Utzschneider Et Cie | Process for obtaining enamelled photographic images on earthenware, porcelain or terracotta objects |
| FR2205492A1 (en) * | 1972-11-03 | 1974-05-31 | Commercial Decal Inc | |
| EP0059276A1 (en) * | 1981-02-27 | 1982-09-08 | Corning Glass Works | Production of decalcomanias and apparatus for the production thereof |
| DE3638170A1 (en) * | 1986-11-08 | 1988-05-11 | Willy Maurer | Process for the decoration of articles made from materials suitable for baking, such as glass, earthenware, ceramic and porcelain, and drawing pencil for a drawing unit |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2828320A1 (en) * | 1978-06-28 | 1980-01-10 | Saueressig Gmbh | Transfer paper photogravure printing press - applies protective coating to rear face between printing mechanism and drying chamber |
-
1992
- 1992-02-05 DE DE4203162A patent/DE4203162A1/en active Granted
- 1992-10-28 DK DK92118362.0T patent/DK0539924T3/en active
- 1992-10-28 AT AT92118362T patent/ATE135637T1/en not_active IP Right Cessation
- 1992-10-28 ES ES92118362T patent/ES2086045T3/en not_active Expired - Lifetime
- 1992-10-28 EP EP92118362A patent/EP0539924B1/en not_active Expired - Lifetime
- 1992-10-28 DE DE59205749T patent/DE59205749D1/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR343180A (en) * | 1904-05-16 | 1904-09-27 | Utzschneider Et Cie | Process for obtaining enamelled photographic images on earthenware, porcelain or terracotta objects |
| FR2205492A1 (en) * | 1972-11-03 | 1974-05-31 | Commercial Decal Inc | |
| EP0059276A1 (en) * | 1981-02-27 | 1982-09-08 | Corning Glass Works | Production of decalcomanias and apparatus for the production thereof |
| DE3638170A1 (en) * | 1986-11-08 | 1988-05-11 | Willy Maurer | Process for the decoration of articles made from materials suitable for baking, such as glass, earthenware, ceramic and porcelain, and drawing pencil for a drawing unit |
Non-Patent Citations (2)
| Title |
|---|
| PATENT ABSTRACTS OF JAPAN vol. 005, no. 054 (C-050)15. April 1981 & JP-A-56 005 359 ( NIPPON SHEET GLASS CO LTD ) 20. Januar 1981 * |
| PATENT ABSTRACTS OF JAPAN vol. 005, no. 127 (M-083)12. August 1981 & JP-A-56 063 486 ( SHIN ETSU CHEM CO LTD ) 30. Mai 1981 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995015266A1 (en) * | 1993-12-02 | 1995-06-08 | Cookson Matthey Print Limited | Method of producing transfer sheets |
| EP0657309A1 (en) * | 1993-12-02 | 1995-06-14 | Cookson Matthey Print Limited | Method of producing transfer sheets |
| WO1996001745A1 (en) * | 1994-07-12 | 1996-01-25 | F. Xaver Leipold Gmbh & Co. Kg | Process for making ceramic transfer images by offset printing |
| AU681977B2 (en) * | 1994-07-12 | 1997-09-11 | F. Xaver Leipold Gmbh & Co. Kg | Process for making ceramic transfer images by offset printing |
| WO1998055327A1 (en) * | 1997-06-04 | 1998-12-10 | University Of The West Of England, Bristol | Printing onto a heat-resistant base |
| GB2340791A (en) * | 1997-06-04 | 2000-03-01 | Univ Bristol | Printing onto a heat-resistant base |
| GB2340791B (en) * | 1997-06-04 | 2001-05-09 | Univ Bristol | Printing onto a heat-resistant base |
| EP1369263A1 (en) * | 2002-05-31 | 2003-12-10 | Tecno-Europa S.r.l. | Method and processing unit for producing decorated sheets for decorating ceramic articles |
| CN107336535A (en) * | 2017-07-24 | 2017-11-10 | 青州新华包装制品有限公司 | A kind of printing process of laser packaging product and the all-in-one using this method |
Also Published As
| Publication number | Publication date |
|---|---|
| DE4203162C2 (en) | 1993-08-19 |
| ES2086045T3 (en) | 1996-06-16 |
| DE59205749D1 (en) | 1996-04-25 |
| DK0539924T3 (en) | 1996-04-15 |
| DE4203162A1 (en) | 1993-05-06 |
| EP0539924B1 (en) | 1996-03-20 |
| ATE135637T1 (en) | 1996-04-15 |
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