EP1101623A2 - Recording material for inkjet printing - Google Patents

Recording material for inkjet printing Download PDF

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Publication number
EP1101623A2
EP1101623A2 EP00123910A EP00123910A EP1101623A2 EP 1101623 A2 EP1101623 A2 EP 1101623A2 EP 00123910 A EP00123910 A EP 00123910A EP 00123910 A EP00123910 A EP 00123910A EP 1101623 A2 EP1101623 A2 EP 1101623A2
Authority
EP
European Patent Office
Prior art keywords
base paper
ink
formaldehyde
paper according
recording material
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
Application number
EP00123910A
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German (de)
French (fr)
Other versions
EP1101623A3 (en
EP1101623B1 (en
Inventor
Hartmut Dr.-Ing. Schulz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Felix Schoeller Jr Foto und Spezialpapiere GmbH
Original Assignee
Felix Schoeller Jr Foto und Spezialpapiere GmbH
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Publication of EP1101623A2 publication Critical patent/EP1101623A2/en
Publication of EP1101623A3 publication Critical patent/EP1101623A3/en
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Publication of EP1101623B1 publication Critical patent/EP1101623B1/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/52—Macromolecular coatings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/502—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording characterised by structural details, e.g. multilayer materials
    • B41M5/508—Supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/502—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording characterised by structural details, e.g. multilayer materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/52—Macromolecular coatings
    • B41M5/5218—Macromolecular coatings characterised by inorganic additives, e.g. pigments, clays

Definitions

  • the invention relates to an ink jet. Recording material with a for this purpose novel base paper.
  • the ink jet recording process becomes tiny Ink droplets with the help of different, already several times techniques described on a recording material brought and taken up by this.
  • the recording material is different Requirements such as high color density of the printed Dots, fast ink absorption and related adequate smudge resistance, a not over that extent of dye diffusion in Transverse direction of the printed dots as well as a small one Mottle and high water resistance.
  • Ink jet recording materials consist of one Backing material, one arranged thereon Ink-receiving layer and possibly other Auxiliary layers.
  • Ink-jet printer for the production of photo-like prints use inks with a high proportion of water as Solvent.
  • inks with a high proportion of water as Solvent.
  • a ripple in the transverse direction (cockle).
  • This Ripple leads to a contact of the Recording material with the print head and has one Deterioration of the printed image. Besides, can the head contact to damage the Lead receiving material. It is therefore necessary for that Manufacture of photo-like ink-jet prints Use recording material in which the Base paper has a high dimensional stability and thus is able to use a large amount of water to record without showing the ripple mentioned above.
  • a receiving material is known from JP 06-262845 A, whose paper base contains a hardwood pulp and has a sizing of starch and alkyl ketene dimer.
  • the used paper is said to have good absorbency and have printed dot uniformity.
  • the disadvantage of this receiving material is that insufficient dimensional stability (ripple) with high Water absorption.
  • JP 11-099737 Ink jet paper can be solved, which is next to a Ink receiving layer at least one other, so-called Carrier layer contains that from a water-insoluble Resin such as polyethylene or polypropylene.
  • Carrier layer contains that from a water-insoluble Resin such as polyethylene or polypropylene.
  • the long drying time of the printed is disadvantageous Recording paper.
  • the object of the invention is a recording material to provide for the ink jet printing process, the one good dimensional stability and high Has water absorption capacity and in addition to high color density, excellent smudge resistance and has good water resistance.
  • a base paper free of bulk sizing agent and containing 5 to 55% by weight of a filler and impregnated with an impregnating resin the resin uptake being adjusted such that the base paper on the back has a liquid absorption of at most 20 g / m 2 , preferably but has 3 to 6 g / m 2 .
  • the back of the base paper is the side opposite the image-bearing side.
  • the invention further relates to an ink jet recording material with the previously described Base paper as a base and at least one on the Front side ink-receiving layer. Between the base and the ink-receiving layer and on the Ink-receiving layer can be arranged further layers his.
  • the filler contained in the base paper can be a Titanium dioxide, zinc sulfide, calcium carbonate, kaolin, talc, Clay or mixtures of these fillers.
  • a Titanium dioxide, zinc sulfide, calcium carbonate, kaolin, talc, Clay or mixtures of these fillers.
  • the Filler content is 5 to 55% by weight, preferably 20 or 25 to 50% by weight.
  • Softwood cellulose long fiber cellulose
  • hardwood cellulose short fiber cellulose
  • Softwood cellulose long fiber cellulose
  • hardwood cellulose short fiber cellulose
  • the fiber length after the milling process should preferably be 0.6 to 1.2 mm.
  • a eucalyptus pulp or a mixture of eucalyptus and softwood pulp is used.
  • the pulp suspension can also contain wet strength agents such as Polyamide / polyamine-epichlorohydrin resin, Retention aids such as quaternary polyammonium salts, Defoamers, penetration accelerators such as saccharides and other aids are added.
  • wet strength agents such as Polyamide / polyamine-epichlorohydrin resin, Retention aids such as quaternary polyammonium salts, Defoamers, penetration accelerators such as saccharides and other aids are added.
  • Base papers do not have any sizing agents that are common be used for mass sizing.
  • this contains Recording material a so-called one-sided smooth Base paper.
  • the one-sided smooth base paper is preferably made on a Yankee paper machine, the long side of the paper web using a heated cylinder is smoothed. Through the long The contact time of the paper with the cylinder can be one closed surface are created, which is a smoothness of 1000 ml / sec, measured according to Bendtson, not should fall below.
  • a open on both sides i.e. unsmoothed base paper can only be used after impregnation smoothed on one or both sides in a calender can be.
  • the resin is a common as Impregnating resin used in the paper industry. It can be selected from the group of diallyl phthalates, Epoxy resins, urea-formaldehyde resins, uric acid-acrylic acid ester copolyesters, Melamine-formaldehyde resins, Melamine-phenol-formaldehyde resins, phenol-formaldehyde resins, Poly (meth) acrylates or unsaturated polyester resins.
  • the coating composition contains a mixture of Acrylic acid ester and urea-formaldehyde resin. Especially good results are with a mix ratio (Mass) acrylic acid ester / urea formaldehyde resin from To achieve 1:10 to 10: 1.
  • the impregnation with the resin can be carried out "in-line” in the paper machine in a glue box or "off-line” outside the paper machine in a size press or an impregnation system.
  • the base paper can be impregnated from the front or from the back or from both sides, the resin penetrating into the interior of the base paper.
  • the resin absorption of the paper is adjusted so that the impregnated base paper has a liquid absorption of at most 20 g / m 2 , preferably 3 to 6 g / m 2 , on the back.
  • the amount of the resin (impregnating agent) can be 2 to 25 g / m 2 , preferably 5 to 8 g / m 2 .
  • any ink receiving layer can be applied.
  • These are mostly hydrophilic Coatings that are water soluble or contain water-dispersible polymers, for example Polyvinyl alcohol, cationic polyvinyl alcohol, Polyvinylpyrrolidone, polyvinyl acetate, starch, gelatin, Casein or carboxymethyl cellulose.
  • the Ink receiving layer can additionally pigments and cationic substances for fixing the ink dyes contain.
  • the ink-receiving layer contains a polyvinyl alcohol or a mixture of polyvinyl alcohol and an acrylic acid ester homopolymer and / or copolymer.
  • the ink-receiving layer may contain a cationic dye fixative and a pigment.
  • the application weight of the ink-receiving layer is 2 to 20 g / m 2 , in particular 6 to 15 g / m 2 .
  • the ink-receiving layer can be applied using the usual methods and air brush or roller doctor metering.
  • the recording paper can contain an additional polymer layer arranged on the receiving layer.
  • the polymer contained in this layer has a Shore hardness (D)> 50 (ASTM D 2240).
  • An acrylic acid ester homopolymer and / or copolymer is particularly suitable.
  • the application weight of the layer is 1 to 10 g / m 2 , in particular 2 to 6 g / m 2 .
  • a mixture of 90% by weight hardwood sulfate pulp and 10% by weight of softwood sulfate pulp was used in one Material density of 4% up to a freeness of 42 ° SR ground. Then 5% by weight was added. Polyamide / polyamine-epichlorohydrin resin and 25% by weight of one Pigment mixture of titanium dioxide (rutile form) and kaolin in a mixing ratio of 1: 1. The weights of the Additives relate to the pulp.
  • a raw paper with a basis weight of 100 g / m 2 and a thickness of 120 ⁇ m was produced from this mixture.
  • the paper which had an air permeability of 8 Gurley seconds per 100 ml, was impregnated with the following impregnating agent: Acrylate / styrene copolymer (47% aqueous dispersion) (Primal® E-2556) 33% by weight Urea-formaldehyde (50% aqueous solution) (Urecoll® TS) 33% by weight Defoamer (OEKOFOAM® -E 190) 1% by weight water 33% by weight
  • the impregnation was carried out in the paper machine with the help of a glue box.
  • the application weights are listed in Table 1 and refer to the dried mass. Table 1 also shows the liquid absorption measured from the back of the impregnated base paper according to DIN 53132. example Application weight, g / m 2 Liquid intake, g / m 2 B1 8th 4th B2 12th 3rd B3 18th 4th
  • the base papers produced according to the examples were coated with an ink receiving layer with the following composition: Polyvinyl alcohol, 20% aqueous solution (Mowiol® 20-98) 760 g Styrene copolymer, 20% dispersion (Basoplast® 265 D) 170 g Butanol 70 g
  • the papers were coated with a doctor knife.
  • the application weight of the ink-receiving layer was 10 g / m 2 for all papers.
  • the papers provided with the ink-receiving layer were coated with a lacquer layer with the following composition, based on the weight of the dried layer, in an amount of 3 g / m 2 : n-butyl acrylate / styrene copolymer (50% aqueous dispersion-Acronal® S 305 D) 95% by weight Crosslinking agent 5% by weight
  • the base paper produced according to Example 1 was without Impregnation with the coating composition according to the invention coated with the ink receiving layer from Example 1.
  • a raw paper with a basis weight of 100 g / m 2 was produced from a cellulose suspension with hardwood cellulose fibers, 25% by weight calcium carbonate, 0.8% by weight cationic starch and 0.5% by weight alkylketene dimer (quantitative data based on the mass of the Pulp).
  • the base paper was then surface-sized with starch and provided with an ink-receiving layer which contains 80% by weight of silica and 20% by weight of polyvinyl alcohol.
  • the recording papers according to the invention were with an inkjet printer HP Deskjet ® 550C from the company Hewlett Packard printed. On the printed papers were the Cockle behavior, the color density, the Smudge resistance, the water resistance and the Water absorption capacity checked.
  • the color density was measured using a Gretag densitometer Colors cyan, magenta, yellow and black in reflected light measured.
  • the paper to be tested was placed on a laid flat base and the flatness of the paper visually with the notes 1 to 5 (very good to very bad) judged.
  • the printed papers were at 25 ° C for one minute put warm water and dried. The color density was measured before and after watering. It is stated remaining color density in percent.
  • test results are summarized in Table 2.
  • example Color density Water resistance cockle Drying cyan magenta yellow black cyan magenta yellow black 1 2.4 2.0 1.9 2.1 98.6 81.5 98.1 98.0 1 ⁇ 10 sec 2 2.3 2.0 1.9 2.2 98.5 83.3 98.5 98.1 1 ⁇ 10 sec 3rd 2.4 2.0 1.9 2.1 99.5 82.0 98.5 98.5 1 ⁇ 10 sec V1 0.8 0.7 0.6 0.8 - - - - 1 ⁇ 10 sec V2 2.4 1.9 1.8 2.2 96.0 80.1 97.6 97.7 5 ⁇ 10 sec

Landscapes

  • Ink Jet Recording Methods And Recording Media Thereof (AREA)
  • Paper (AREA)
  • Ink Jet (AREA)
  • Duplication Or Marking (AREA)
  • Materials For Medical Uses (AREA)

Abstract

Ink jet printing base paper, comprises filler (5-55 wt.%) and paper, free of size and impregnated such that the liquid uptake of the reverse side is at most 20 g/m<2>.

Description

Die Erfindung betrifft ein Tintenstrahl(Ink-Jet) - Aufzeichnungsmaterial mit einem für diesen Zweck neuartigen Basispapier.The invention relates to an ink jet. Recording material with a for this purpose novel base paper.

Beim Ink-Jet-Aufzeichnungsverfahren werden winzige Tintentröpfchen mit Hilfe verschiedener, bereits mehrfach beschriebener Techniken auf ein Aufzeichnungsmaterial gebracht und von diesem aufgenommen.The ink jet recording process becomes tiny Ink droplets with the help of different, already several times techniques described on a recording material brought and taken up by this.

An das Aufzeichnungsmaterial werden unterschiedliche Anforderungen gestellt wie hohe Farbdichte der gedruckten Punkte, eine schnelle Tintenaufnahme und damit verbundene ausreichende Wischfestigkeit, eine nicht über das notwendige Ausmaß hinausgehende Farbstoffdiffusion in Querrichtung der gedruckten Punkte sowie ein geringer Mottle und eine hohe Wasserfestigkeit.The recording material is different Requirements such as high color density of the printed Dots, fast ink absorption and related adequate smudge resistance, a not over that extent of dye diffusion in Transverse direction of the printed dots as well as a small one Mottle and high water resistance.

Tintenstrahl-Aufzeichnungsmaterialien bestehen aus einem Trägermaterial, einer darauf angeordneten Tintenaufnahmeschicht und gegebenenfalls weiteren Hilfsschichten.Ink jet recording materials consist of one Backing material, one arranged thereon Ink-receiving layer and possibly other Auxiliary layers.

Ink-Jet-Drucker zur Herstellung fotoähnlicher Drucke benutzen Tinten mit einem hohen Anteil Wasser als Lösungsmittel. Bei Benutzung herkömmlicher Ink-Jet-Papiere tritt durch den hohen Wassergehalt, der durch die Papiere tritt durch den hohen Wassergehalt, der durch die Tintenaufnahmeschicht in die Papierunterlage eindringt, eine Welligkeit in Querrichtung (cockle) auf. Diese Welligkeit führt zu einem Kontakt des Aufzeichnungsmaterials mit dem Druckkopf und hat eine Verschlechterung des Druckbilds zur Folge. Außerdem kann der Kopfkontakt zu einer Beschädigung des Empfangsmaterials führen. Es ist daher notwendig, für die Herstellung fotoähnlicher Ink-Jet-Drucke ein Aufzeichnungsmaterial einzusetzen, bei dem das Basispapier eine hohe Dimensionsstabilität aufweist und somit in der Lage ist, eine große Wassermenge aufzunehmen, ohne die oben erwähnte Welligkeit zu zeigen.Ink-jet printer for the production of photo-like prints use inks with a high proportion of water as Solvent. When using conventional ink jet papers occurs due to the high water content caused by the Papers occurs due to the high water content caused by the Ink absorption layer penetrates into the paper base, a ripple in the transverse direction (cockle). This Ripple leads to a contact of the Recording material with the print head and has one Deterioration of the printed image. Besides, can the head contact to damage the Lead receiving material. It is therefore necessary for that Manufacture of photo-like ink-jet prints Use recording material in which the Base paper has a high dimensional stability and thus is able to use a large amount of water to record without showing the ripple mentioned above.

Aus der JP 06-262845 A ist ein Empfangsmaterial bekannt, dessen Papierträger einen Laubholz-Zellstoff enthält und eine Leimung aus Stärke und Alkylketendimer aufweist. Das beanspruchte Papier soll eine gute Absorptionsfähigkeit und eine Gleichmäßigkeit der gedruckten Punkte aufweisen. Nachteilig jedoch an diesem Empfangsmaterial ist die unzureichende Dimensionsstabilität (Welligkeit) bei hoher Wasseraufnahme.A receiving material is known from JP 06-262845 A, whose paper base contains a hardwood pulp and has a sizing of starch and alkyl ketene dimer. The used paper is said to have good absorbency and have printed dot uniformity. However, the disadvantage of this receiving material is that insufficient dimensional stability (ripple) with high Water absorption.

Das gleiche Problem der unzureichenden Dimensionsstabilität bei hoher Wasseraufnahme ist bei einem in der JP 08-258399 A beschriebenen Aufzeichnungspapier zu beobachten, welches ein Calciumcarbonat mit spindelförmigen Partikeln und neutrale Leimungsmittel enthält.The same problem of inadequate Dimensional stability with high water absorption is at one described in JP 08-258399 A. Watching paper, which one Calcium carbonate with spindle - shaped particles and contains neutral sizing agents.

Das Cockle-Problem soll in der JP 11-099737 durch ein Ink-Jet-Papier gelöst werden, welches neben einer Tintenaufnahmeschicht mindestens eine weitere, sogenannte Trägerschicht enthält, die aus einem wasserunlöslichen Harz wie Polyethylen oder Polypropylen besteht. Nachteilig ist die lange Trocknungszeit des bedruckten Aufzeichnungspapiers.The Cockle problem is said to exist in JP 11-099737 Ink jet paper can be solved, which is next to a Ink receiving layer at least one other, so-called Carrier layer contains that from a water-insoluble Resin such as polyethylene or polypropylene. The long drying time of the printed is disadvantageous Recording paper.

Aufgabe der Erfindung ist es, ein Aufzeichnungsmaterial für das Ink-Jet-Druckverfahren bereitzustellen, das eine gute Dimensionsstabilität und hohe Wasseraufnahmefähigkeit aufweist und darüber hinaus neben hoher Farbdichte eine ausgezeichnete Wischfestigkeit und gute Wasserfestigkeit aufweist.The object of the invention is a recording material to provide for the ink jet printing process, the one good dimensional stability and high Has water absorption capacity and in addition to high color density, excellent smudge resistance and has good water resistance.

Diese Aufgabe wird durch ein von Masseleimungsmittel freies, 5 bis 55 Gew.% eines Füllstoffs enthaltendes und mit einem Tränkharz imprägniertem Basispapier gelöst, wobei die Harzaufnahme so eingestellt ist, daß das Basispapier auf der Rückseite eine Flüssigkeitsaufnahme von höchstens 20 g/m2, vorzugsweise aber 3 bis 6 g/m2 aufweist. Die Rückseite des Basispapiers ist die der bildtragenden Seite gegenüber liegende Seite.This object is achieved by a base paper free of bulk sizing agent and containing 5 to 55% by weight of a filler and impregnated with an impregnating resin, the resin uptake being adjusted such that the base paper on the back has a liquid absorption of at most 20 g / m 2 , preferably but has 3 to 6 g / m 2 . The back of the base paper is the side opposite the image-bearing side.

Gegenstand der Erfindung ist ferner ein Tintenstrahl-Aufzeichnungsmaterial mit dem zuvor beschriebenen Basispapier als Unterlage und mindestens einer auf der Vorderseite angeordneten Tintenaufnahmeschicht. Zwischen der Unterlage und der Tintenaufnahmeschicht und auf der Tintenaufnahmeschicht können weitere Schichten angeordnet sein.The invention further relates to an ink jet recording material with the previously described Base paper as a base and at least one on the Front side ink-receiving layer. Between the base and the ink-receiving layer and on the Ink-receiving layer can be arranged further layers his.

Der im Rohpapier enthaltene Füllstoff kann ein Titandioxid, Zinksulfid, Calciumcarbonat, Kaolin, Talkum, Clay oder Gemische dieser Füllstoffe sein. In einer bevorzugten Ausführungsform wird ein Gemisch aus Titandioxid und Kaolin in einem Mischungsverhältnis 1:10 bis 10:1 (Masse) eingesetzt. Besonders gute Ergebnisse werden bei einem Mischungsverhältnis von 1:1 erzielt. Der Füllstoffanteil beträgt 5 bis 55 Gew.%, vorzugsweise 20 oder 25 bis 50 Gew.%.The filler contained in the base paper can be a Titanium dioxide, zinc sulfide, calcium carbonate, kaolin, talc, Clay or mixtures of these fillers. In a preferred embodiment is a mixture of Titanium dioxide and kaolin in a mixture ratio of 1:10 up to 10: 1 (mass) used. Particularly good results are achieved with a mixing ratio of 1: 1. The Filler content is 5 to 55% by weight, preferably 20 or 25 to 50% by weight.

Zur Herstellung des erfindungsgemäßen Basispapiers können Nadelholz-Zellstoffe (Langfaser-Zellstoffe) oder Laubholz-Zellstoffe (Kurzfaser-Zellstoffe) verwendet werden. Bevorzugt wird ein Zellstoff oder Zellstoff-Gemisch mit einem spezifischen Volumen von 1,4 bis 2,0 cm3/g, insbesondere 1,4 bis 1,6 cm3/g (bei einem Mahlgrad von 20 bis 35°SR). Die Faserlänge nach dem Mahlvorgang sollte vorzugsweise 0,6 bis 1,2 mm betragen. In einer besonderen Ausgestaltung der Erfindung wird ein Eukalyptus-Zellstoff oder ein Gemisch aus Eukalyptus- und Nadelholz-Zellstoff eingesetzt.Softwood cellulose (long fiber cellulose) or hardwood cellulose (short fiber cellulose) can be used to produce the base paper according to the invention. A pulp or cellulose mixture with a specific volume of 1.4 to 2.0 cm 3 / g, in particular 1.4 to 1.6 cm 3 / g (at a freeness of 20 to 35 ° SR) is preferred. The fiber length after the milling process should preferably be 0.6 to 1.2 mm. In a special embodiment of the invention, a eucalyptus pulp or a mixture of eucalyptus and softwood pulp is used.

Der Zellstoffsuspension können außerdem Naßfestmittel wie Polyamid/Polyamin-Epichlorhydrin-Harz, Retentionshilfsmittel wie quaternäre Polyammoniumsalze, Entschäumer, Penetrationsbeschleuniger wie Saccharide und andere Hilfsmittel zugesetzt werden. Im Vergleich zu herkömmlichen Basispapieren für Ink-Jet-Aufzeichnungsmaterialien weisen die erfindungsgemäßen Rohpapiere keine Leimungsmittel auf, die üblicherweise zur Masseleimung eingesetzt werden.The pulp suspension can also contain wet strength agents such as Polyamide / polyamine-epichlorohydrin resin, Retention aids such as quaternary polyammonium salts, Defoamers, penetration accelerators such as saccharides and other aids are added. Compared to conventional base papers for ink jet recording materials point the invention Base papers do not have any sizing agents that are common be used for mass sizing.

Gemäß einer Ausführungsform der Erfindung enthält das Aufzeichnungsmaterial ein sogenanntes einseitig glattes Rohpapier. Das einseitig glatte Rohpapier wird vorzugsweise auf einer Yankee-Papiermaschine hergestellt, wobei die Langsiebseite der Papierbahn mit Hilfe eines beheizten Zylinders geglättet wird. Durch die lange Kontaktzeit des Papiers mit dem Zylinder kann eine geschlossene Oberfläche erzeugt werden, die eine Glätte von 1000 ml/sec, gemessen nach Bendtson, nicht unterschreiten sollte.According to one embodiment of the invention, this contains Recording material a so-called one-sided smooth Base paper. The one-sided smooth base paper is preferably made on a Yankee paper machine, the long side of the paper web using a heated cylinder is smoothed. Through the long The contact time of the paper with the cylinder can be one closed surface are created, which is a smoothness of 1000 ml / sec, measured according to Bendtson, not should fall below.

In weiteren Ausgestaltungen der Erfindung kann auch ein beidseitig offenes, d.h. nicht geglättetes Rohpapier eingesetzt werden, das erst nach dem Imprägnieren einseitig oder beidseitig in einem Kalander geglättet werden kann.In further refinements of the invention, a open on both sides, i.e. unsmoothed base paper can only be used after impregnation smoothed on one or both sides in a calender can be.

Das Harz (Imprägniermittel) ist ein übliches als Tränkharz in der Papierindustrie verwendetes Harz. Es kann ausgewählt sein aus der Gruppe der Diallylphthalate, Epoxidharze, Harnstoff-Formaldehyd-Harze, Harnsäure-Acrylsäureester-Copolyester, Melamin-Formaldehyd-Harze, Melamin-Phenol-Formaldehyd-Harze, Phenol-Formaldehyd-Harze, Poly(meth)acrylate oder ungesättigter Polyester-Harze. In einer besonderen Ausgestaltung der Erfindung enthält die Beschichtungsmasse ein Gemisch aus einem Acrylsäureester und Harnstoff-Formaldehyd-Harz. Besonders gute Ergebnisse sind bei einem Mischungsverhältnis (Masse) Acrylsäureester/ Harnstoff-Formaldehyd-Harz von 1:10 bis 10:1 zu erzielen.The resin (impregnating agent) is a common as Impregnating resin used in the paper industry. It can be selected from the group of diallyl phthalates, Epoxy resins, urea-formaldehyde resins, uric acid-acrylic acid ester copolyesters, Melamine-formaldehyde resins, Melamine-phenol-formaldehyde resins, phenol-formaldehyde resins, Poly (meth) acrylates or unsaturated polyester resins. In a special embodiment of the invention the coating composition contains a mixture of Acrylic acid ester and urea-formaldehyde resin. Especially good results are with a mix ratio (Mass) acrylic acid ester / urea formaldehyde resin from To achieve 1:10 to 10: 1.

Die Imprägnierung mit dem Harz kann "in-line" in der Papiermaschine in einem Leimkasten oder "off-line" außerhalb der Papiermaschine in einer Leimpresse oder einer Imprägnieranlage durchgeführt werden. Das Rohpapier kann von der Vorderseite oder von der Rückseite oder aber von beiden Seiten imprägniert werden, wobei das Harz in das Innere des Rohpapiers eindringt. Die Harzaufnahme des Papiers ist so eingestellt, daß das imprägnierte Rohpapier auf der Rückseite eine Flüssigkeitsaufnahme von höchstens 20 g/m2, vorzugsweise 3 bis 6 g/m2, aufweist. Die Menge des Harzes (Imprägniermittel) kann 2 bis 25 g/m2, vorzugsweise 5 bis 8 g/m2 betragen.The impregnation with the resin can be carried out "in-line" in the paper machine in a glue box or "off-line" outside the paper machine in a size press or an impregnation system. The base paper can be impregnated from the front or from the back or from both sides, the resin penetrating into the interior of the base paper. The resin absorption of the paper is adjusted so that the impregnated base paper has a liquid absorption of at most 20 g / m 2 , preferably 3 to 6 g / m 2 , on the back. The amount of the resin (impregnating agent) can be 2 to 25 g / m 2 , preferably 5 to 8 g / m 2 .

Auf das erfindungsgemäße Basispapier kann grundsätzlich jede beliebige Tintenaufnahmeschicht aufgetragen werden. Hierbei handelt es sich meistens um hydrophile Beschichtungen, die wasserlösliche oder wasserdispergierbare Polymere enthalten, beispielsweise Polyvinylalkohol, kationischer Polyvinylalkohol, Polyvinylpyrrolidon, Polyvinylacetat, Stärke, Gelatine, Kasein oder Carboxymethylcellulose. Die Tintenaufnahmeschicht kann zusätzlich Pigmente und kationische Substanzen zur Fixierung der Tintenfarbstoffe enthalten.Basically, on the base paper according to the invention any ink receiving layer can be applied. These are mostly hydrophilic Coatings that are water soluble or contain water-dispersible polymers, for example Polyvinyl alcohol, cationic polyvinyl alcohol, Polyvinylpyrrolidone, polyvinyl acetate, starch, gelatin, Casein or carboxymethyl cellulose. The Ink receiving layer can additionally pigments and cationic substances for fixing the ink dyes contain.

In einer besonderen Ausgestaltung der Erfindung enthält die Tintenaufnahmeschicht einen Polyvinylalkohol oder eine Mischung aus Polyvinylalkohol und einem Acrylsäureester-Homopolymer und/oder -Copolymer. In einer anderen Ausgestaltung der Erfindung kann die Tintenaufnahmeschicht ein kationisches Farbstoffixiermittel und ein Pigment enthalten. Das Auftragsgewicht der Tintenaufnahmeschicht beträgt 2 bis 20 g/m2, insbesondere 6 bis 15 g/m2. Die Tintenaufnahmeschicht kann mit den üblichen Verfahren und Luftbürsten- oder Rollrakeldosierung aufgetragen werden.In a particular embodiment of the invention, the ink-receiving layer contains a polyvinyl alcohol or a mixture of polyvinyl alcohol and an acrylic acid ester homopolymer and / or copolymer. In another aspect of the invention, the ink-receiving layer may contain a cationic dye fixative and a pigment. The application weight of the ink-receiving layer is 2 to 20 g / m 2 , in particular 6 to 15 g / m 2 . The ink-receiving layer can be applied using the usual methods and air brush or roller doctor metering.

In einer besonderen Ausführungsform der Erfindung kann das Aufzeichnungspapier eine zusätzliche, auf der Empfangsschicht angeordnete Polymerschicht enthalten. Das in dieser Schicht enthaltene Polymer weist eine Shore-Härte (D) > 50 auf (ASTM D 2240). Besonders geeignet ist ein Acrylsäureester-Homopolymer und/oder -Copolymer. Das Auftragsgewicht der Schicht beträgt 1 bis 10 g/m2, insbesondere 2 bis 6 g/m2.In a particular embodiment of the invention, the recording paper can contain an additional polymer layer arranged on the receiving layer. The polymer contained in this layer has a Shore hardness (D)> 50 (ASTM D 2240). An acrylic acid ester homopolymer and / or copolymer is particularly suitable. The application weight of the layer is 1 to 10 g / m 2 , in particular 2 to 6 g / m 2 .

Die Erfindung wird durch die folgenden Beispiele näher erläutert.The invention is illustrated by the following examples explained.

Beispiele 1 bis 3Examples 1 to 3

Eine Mischung aus 90 Gew.% Laubholzsulfat-Zellstoff und 10 Gew.% Nadelholzsulfat-Zellstoff wurde bei einer Stoffdichte von 4% bis zu einem Mahlgrad von 42 °SR gemahlen. Anschließend erfolgte die Zugabe von 5 Gew.% Polyamid/Polyamin-Epichlorhydrin-Harz und 25 Gew.% eines Pigment-Gemisches aus Titandioxid (Rutil-Form) und Kaolin in einem Mischverhältnis von 1:1. Die Gewichtsangaben der Zusätze beziehen sich auf den Zellstoff.A mixture of 90% by weight hardwood sulfate pulp and 10% by weight of softwood sulfate pulp was used in one Material density of 4% up to a freeness of 42 ° SR ground. Then 5% by weight was added. Polyamide / polyamine-epichlorohydrin resin and 25% by weight of one Pigment mixture of titanium dioxide (rutile form) and kaolin in a mixing ratio of 1: 1. The weights of the Additives relate to the pulp.

Aus dieser Mischung wurde ein Rohpapier mit einem Flächengewicht von 100 g/m2 und einer Dicke von 120 µm gefertigt. Das eine Luftdurchlässigkeit von 8 Gurley Sekunden je 100 ml aufweisende Papier wurde mit folgendem Imprägniermittel imprägniert: Acrylat/Styrol-Copolymer (47%ige wässrige Dispersion) (Primal® E-2556) 33 Gew.% Harnstoff-Formaldehyd (50%ige wässrige Lösung) (Urecoll® TS) 33 Gew.% Entschäumer (OEKOFOAM® -E 190) 1 Gew.% Wasser 33 Gew.% A raw paper with a basis weight of 100 g / m 2 and a thickness of 120 µm was produced from this mixture. The paper, which had an air permeability of 8 Gurley seconds per 100 ml, was impregnated with the following impregnating agent: Acrylate / styrene copolymer (47% aqueous dispersion) (Primal® E-2556) 33% by weight Urea-formaldehyde (50% aqueous solution) (Urecoll® TS) 33% by weight Defoamer (OEKOFOAM® -E 190) 1% by weight water 33% by weight

Die Imprägnierung erfolgte in der Papiermaschine mit Hilfe eines Leimkastens. Die Auftragsgewichte sind in Tabelle 1 aufgeführt und beziehen sich auf die getrocknete Masse. Ebenfalls in Tabelle 1 genannt ist die von der Rückseite des imprägnierten Basispapiers nach DIN 53132 gemessene Flüssigkeitsaufnahme. Beispiel Auftragsgewicht, g/m2 Flüssigkeitsaufnahme, g/m2 B1 8 4 B2 12 3 B3 18 4 The impregnation was carried out in the paper machine with the help of a glue box. The application weights are listed in Table 1 and refer to the dried mass. Table 1 also shows the liquid absorption measured from the back of the impregnated base paper according to DIN 53132. example Application weight, g / m 2 Liquid intake, g / m 2 B1 8th 4th B2 12th 3rd B3 18th 4th

Die gemäß den Beispielen hergestellten Basispapiere wurden mit einer Tintenaufnahmeschicht mit folgender Zusammensetzung beschichtet: Polyvinylalkohol, 20%ige wäßrige Lösung (Mowiol® 20-98) 760 g Styrol-Copolymer, 20%ige Dispersion (Basoplast® 265 D) 170 g Butanol 70 g The base papers produced according to the examples were coated with an ink receiving layer with the following composition: Polyvinyl alcohol, 20% aqueous solution (Mowiol® 20-98) 760 g Styrene copolymer, 20% dispersion (Basoplast® 265 D) 170 g Butanol 70 g

Die Beschichtung der Papiere erfolgte mittels Rakeldosierung. Das Auftragsgewicht der Tintenaufnahmeschicht betrug bei allen Papieren 10 g/m2.The papers were coated with a doctor knife. The application weight of the ink-receiving layer was 10 g / m 2 for all papers.

In einem weiteren Arbeitsschritt wurden die mit der Tintenaufnahmeschicht versehenen Papiere mit einer Lackschicht mit folgender Zusammensetzung, bezogen auf das Gewicht der getrockneten Schicht, in einer Menge von 3 g/m2 beschichtet: n-Butylacrylat/Styrol-Copolymer (50%ige wässrige Dispersion-Acronal® S 305 D) 95 Gew.% Vernetzungsmittel 5 Gew.% In a further step, the papers provided with the ink-receiving layer were coated with a lacquer layer with the following composition, based on the weight of the dried layer, in an amount of 3 g / m 2 : n-butyl acrylate / styrene copolymer (50% aqueous dispersion-Acronal® S 305 D) 95% by weight Crosslinking agent 5% by weight

Vergleichsbeispiel V1Comparative Example V1

Das gemäß Beispiel 1 hergestellte Rohpapier wurde ohne Imprägnierung mit der erfindunggemäßen Beschichtungsmasse mit der Tintenaufnahmeschicht aus Beispiel 1 beschichtet.The base paper produced according to Example 1 was without Impregnation with the coating composition according to the invention coated with the ink receiving layer from Example 1.

Vergleichsbeispiel V2Comparative example V2

Aus einer Zellstoffsuspension mit Laubholz-Zellstoffasern, 25 Gew.% Calciumcarbonat, 0,8 Gew.% kationischer Stärke und 0,5 Gew.% Alkylketendimer wurde ein Rohpapier mit einem Flächengewicht von 100 g/m2 gefertigt (Mengenangaben bezogen auf die Masse des Zellstoffs). Anschließend wurde das Rohpapier mit Stärke oberflächengeleimt und mit einer Tintenaufnahmeschicht, die 80 Gew.% Kieselsäure und 20 Gew.% Polyvinylalkohol enthält, versehen.A raw paper with a basis weight of 100 g / m 2 was produced from a cellulose suspension with hardwood cellulose fibers, 25% by weight calcium carbonate, 0.8% by weight cationic starch and 0.5% by weight alkylketene dimer (quantitative data based on the mass of the Pulp). The base paper was then surface-sized with starch and provided with an ink-receiving layer which contains 80% by weight of silica and 20% by weight of polyvinyl alcohol.

Prüfung der gemäß Beispiel 1 bis 3 und Vergleichsbeispiel V1 bis V2 hergestellten AufzeichnungspapiereTesting of according to Examples 1 to 3 and comparative example V1 to V2 produced recording papers

Die erfindungsgemäßen Aufzeichnungspapiere wurden mit einem Tintenstrahldrucker HP Deskjet ® 550C der Firma Hewlett Packard bedruckt. An den bedruckten Papieren wurden das Cockle-Verhalten, die Farbdichte, die Wischfestigkeit, die Wasserfestigkeit und die Wasseraufnahmefähigkeit geprüft.The recording papers according to the invention were with an inkjet printer HP Deskjet ® 550C from the company Hewlett Packard printed. On the printed papers were the Cockle behavior, the color density, the Smudge resistance, the water resistance and the Water absorption capacity checked.

FarbdichteColor density

Die Farbdichte wurde mit einem Densitometer Gretag an den Farben Cyan, Magenta, Gelb und Schwarz im Auflicht gemessen.The color density was measured using a Gretag densitometer Colors cyan, magenta, yellow and black in reflected light measured.

Cockle-Verhalten (Welligkeit)Cockle behavior (ripple)

Zur Bestimmung wurde das zu prüfende Papier auf eine ebene Unterlage gelegt und die Planlage des Papiers visuell mit den Noten 1 bis 5 (sehr gut bis sehr schlecht) beurteilt.For the determination, the paper to be tested was placed on a laid flat base and the flatness of the paper visually with the notes 1 to 5 (very good to very bad) judged.

WasserfestigkeitWater resistance

Die bedruckten Papiere wurden eine Minute lang in 25°C warmes Wasser gelegt und getrocknet. Die Farbdichte wurde vor und nach dem Wässern gemessen. Angegeben ist die verbliebene Farbdichte in Prozent. The printed papers were at 25 ° C for one minute put warm water and dried. The color density was measured before and after watering. It is stated remaining color density in percent.

TrocknungsverhaltenDrying behavior

Auf das erfindungsgemäße Aufzeichnungspapier wurde ein DIN-A5-Bild gedruckt. Nach Beendigung des Druckvorgangs wurde das Bild im 10 Sekunden-Intervall leicht mit dem Finger über die Oberfläche gerieben und nach Verwischspuren untersucht. Die Trocknungszeit wurde für die Bereiche ≤10 Sekunden (sehr gut) und 20-30 Sekunden (schlecht) beurteilt.On the recording paper according to the invention was a Printed A5 image. After printing is finished the image became light with the 10 second interval Fingers rubbed over the surface and after Blur marks examined. The drying time was for the ranges ≤10 seconds (very good) and 20-30 seconds (bad) judged.

Die Prüfungsergebnisse sind in Tabelle 2 zusammengestellt. Beispiel Farbdichte Wasserfestigkeit cockle Trocknung cyan magenta gelb schwarz cyan magenta gelb schwarz 1 2,4 2,0 1,9 2,1 98,6 81,5 98,1 98,0 1 <10 sec 2 2,3 2,0 1,9 2,2 98,5 83,3 98,5 98,1 1 <10 sec 3 2,4 2,0 1,9 2,1 99,5 82,0 98,5 98,5 1 <10 sec V1 0,8 0,7 0,6 0,8 - - - - 1 <10 sec V2 2,4 1,9 1,8 2,2 96,0 80,1 97,6 97,7 5 <10 sec The test results are summarized in Table 2. example Color density Water resistance cockle Drying cyan magenta yellow black cyan magenta yellow black 1 2.4 2.0 1.9 2.1 98.6 81.5 98.1 98.0 1 <10 sec 2 2.3 2.0 1.9 2.2 98.5 83.3 98.5 98.1 1 <10 sec 3rd 2.4 2.0 1.9 2.1 99.5 82.0 98.5 98.5 1 <10 sec V1 0.8 0.7 0.6 0.8 - - - - 1 <10 sec V2 2.4 1.9 1.8 2.2 96.0 80.1 97.6 97.7 5 <10 sec

Wie aus der Tabelle ersichtlich, kann bei hohen Farbdichten, guter Wasserfestigkeit und kurzen Trocknungszeiten ein sehr gutes Cockle-Verhalten des Aufzeichnungsmaterials erreicht werden.As can be seen from the table, at high Color densities, good water resistance and short Drying times a very good cockle behavior of the Recording material can be achieved.

Claims (10)

Basispapier für ein Aufzeichnungsmaterial für das Tintenstrahl-Druckverfahren, dadurch gekennzeichnet, daß 5 bis 55 Gew.% eines Füllstoffs enthalten sind, das Papier von Masseleimungsmitteln frei ist und mit einem Imprägniermittel imprägniert ist, wobei die Harzaufnahme aus dem Imprägniermittel so eingestellt ist, daß das Basispapier auf der Rückseite eine Flüssigkeitsaufnahme von höchstens 20 g/m2 aufweist.Base paper for a recording material for the ink jet printing process, characterized in that it contains 5 to 55% by weight of a filler, the paper is free from size sizing agents and is impregnated with an impregnating agent, the resin uptake from the impregnating agent being adjusted so that Base paper on the back has a liquid absorption of at most 20 g / m 2 . Basispapier nach Anspruch 1, dadurch gekennzeichnet, daß die Flüssigkeitsaufnahme auf der Rückseite 3 bis 6 g/m2 beträgt.Base paper according to claim 1, characterized in that the liquid absorption on the back is 3 to 6 g / m 2 . Basispapier nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß der Füllstoff ein Titandioxid, Zinksulfid, Calciumcarbonat, Kaolin, Talkum, Clay oder Gemische davon sein kann.Base paper according to claim 1 or 2, characterized in that the filler can be a titanium dioxide, zinc sulfide, calcium carbonate, kaolin, talc, clay or mixtures thereof. Basispapier nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß der Füllstoff ein Gemisch aus Titandioxid und Kaolin in einem Mischungsverhältnis 1:10 bis 10:1 ist.Base paper according to one of claims 1 to 3, characterized in that the filler is a mixture of titanium dioxide and kaolin in a mixing ratio of 1:10 to 10: 1. Basispapier nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Menge des Imprägniermittels 2 bis 25 g/m2, vorzugsweise 5 bis 8 g/m2 beträgt. Base paper according to one of claims 1 to 4, characterized in that the amount of the impregnating agent is 2 to 25 g / m 2 , preferably 5 to 8 g / m 2 . Basispapier nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß das Imprägniermittel ein Harz aus der Gruppe der Diallylphthalate, Epoxid-, Harnstoff-Formaldehyd-, Melamin-Formaldehyd-, Melamin-Phenol-Formaldehyd-, Phenol-Formaldehyd- oder ungesättigter Polyester-Harze enthält.Base paper according to one of claims 1 to 5, characterized in that the impregnating agent is a resin from the group of the diallyl phthalates, epoxy, urea-formaldehyde, melamine-formaldehyde, melamine-phenol-formaldehyde, phenol-formaldehyde or unsaturated polyester - Contains resins. Basispapier nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß das Imprägniermittel ein Gemisch aus Acrylat und Harnstoff-Formaldehyd-Harz enthält.Base paper according to one of claims 1 to 6, characterized in that the impregnating agent contains a mixture of acrylate and urea-formaldehyde resin. Basispapier nach Anspruch 7, dadurch gekennzeichnet, daß das Mengenverhältnis Acrylat/Harnstoff-Formaldehyd 1:10 bis 10:1 beträgt.Base paper according to claim 7, characterized in that the quantitative ratio of acrylate / urea-formaldehyde is 1:10 to 10: 1. Aufzeichnungsmaterial für das Tintenstrahl-Druckverfahren, enthaltend ein Basispapier nach einem der Ansprüche 1 bis 9 mit mindestens einer Tintenaufzeichnungsschicht und gegebenenfalls weiteren Schichten zwischen dem Basispapier und der Tintenaufnahmeschicht und auf der Tintenaufnahmeschicht.Recording material for the inkjet printing process, containing a base paper according to one of the Claims 1 to 9 with at least one Ink recording layer and optionally other Layers between the base paper and the Ink-receiving layer and on the ink-receiving layer. Aufzeichnungsmaterial nach Anspruch 9, dadurch gekennzeichnet, daß auf der Tintenaufnahmeschicht eine ein Polymer mit einer Shore-Härte >50 (DIN 53505) enthaltende Schutzschicht angeordnet ist.Recording material according to claim 9, characterized in that a protective layer containing a polymer with a Shore hardness> 50 (DIN 53505) is arranged on the ink receiving layer.
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WO2004003293A1 (en) * 2002-06-27 2004-01-08 Upm-Kymmene Oyj Printed substrate and printing method
US7435473B2 (en) 2002-06-27 2008-10-14 Upm-Kymmene Oyj Printed substrate and printing method
EP2865527A1 (en) * 2013-10-22 2015-04-29 Agfa Graphics Nv Manufacturing of decorative surfaces by inkjet
EP2865528A1 (en) * 2013-10-22 2015-04-29 Agfa Graphics Nv Manufacturing of decorative surfaces by inkjet
WO2015059002A1 (en) * 2013-10-22 2015-04-30 Agfa Graphics Nv Manufacturing of decorative surfaces by inkjet
WO2015058974A1 (en) * 2013-10-22 2015-04-30 Agfa Graphics Nv Manufacturing of decorative surfaces by inkjet
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EP2979887A1 (en) * 2013-10-22 2016-02-03 Agfa Graphics Nv Manufacturing of decorative surfaces by inkjet
CN105658436A (en) * 2013-10-22 2016-06-08 爱克发印艺公司 Manufacturing of decorative surfaces by inkjet
US9724932B2 (en) 2013-10-22 2017-08-08 Agfa Graphics Nv Manufacturing of decorative surfaces by inkjet
EP2865528B1 (en) 2013-10-22 2018-01-31 Agfa Nv Manufacturing of decorative surfaces by inkjet
EP3293013A1 (en) * 2013-10-22 2018-03-14 Agfa Nv Manufacturing of decorative surfaces by inkjet
US10022956B2 (en) 2013-10-22 2018-07-17 Agfa Nv Manufacturing of decorative surfaces by inkjet
CN109572260A (en) * 2013-10-22 2019-04-05 爱克发有限公司 Decorative surface is produced by ink-jet
US11400701B2 (en) 2013-10-22 2022-08-02 Agfa Nv Manufacturing of decorative surfaces by inkjet
EP3848422B1 (en) 2017-08-22 2022-11-30 Agfa Nv Manufacturing decorative panels

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US6599592B1 (en) 2003-07-29
DE19955081C1 (en) 2001-08-09
EP1101623A3 (en) 2002-04-03
PT1101623E (en) 2005-11-30
CN1182977C (en) 2005-01-05
CN1295932A (en) 2001-05-23
CA2325237A1 (en) 2001-05-15
BR0005397B1 (en) 2010-06-15
BR0005397A (en) 2001-09-18
ES2246209T3 (en) 2006-02-16
CA2325237C (en) 2005-06-14
DE50010911D1 (en) 2005-09-15
EP1101623B1 (en) 2005-08-10
DK1101623T3 (en) 2005-12-12
JP2001199157A (en) 2001-07-24
PL343882A1 (en) 2001-05-21
ATE301549T1 (en) 2005-08-15
PL196450B1 (en) 2008-01-31

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