EP0935021A1 - Absorbent household paper - Google Patents

Absorbent household paper Download PDF

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Publication number
EP0935021A1
EP0935021A1 EP99400269A EP99400269A EP0935021A1 EP 0935021 A1 EP0935021 A1 EP 0935021A1 EP 99400269 A EP99400269 A EP 99400269A EP 99400269 A EP99400269 A EP 99400269A EP 0935021 A1 EP0935021 A1 EP 0935021A1
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EP
European Patent Office
Prior art keywords
fold
ply
protrusions
protuberances
complex sheet
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EP99400269A
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German (de)
French (fr)
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EP0935021B1 (en
Inventor
Pierre Graff
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Essity Operations France SAS
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Fort James France
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B31—MAKING ARTICLES OF PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER; WORKING PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER
    • B31F—MECHANICAL WORKING OR DEFORMATION OF PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER
    • B31F1/00—Mechanical deformation without removing material, e.g. in combination with laminating
    • B31F1/07—Embossing, i.e. producing impressions formed by locally deep-drawing, e.g. using rolls provided with complementary profiles
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/30—Multi-ply
    • D21H27/40—Multi-ply at least one of the sheets being non-planar, e.g. crêped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B31—MAKING ARTICLES OF PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER; WORKING PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER
    • B31F—MECHANICAL WORKING OR DEFORMATION OF PAPER, CARDBOARD OR MATERIAL WORKED IN A MANNER ANALOGOUS TO PAPER
    • B31F2201/00—Mechanical deformation of paper or cardboard without removing material
    • B31F2201/07—Embossing
    • B31F2201/0707—Embossing by tools working continuously
    • B31F2201/0715—The tools being rollers
    • B31F2201/0723—Characteristics of the rollers
    • B31F2201/0733—Pattern
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/02—Patterned paper
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24355—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
    • Y10T428/24446—Wrinkled, creased, crinkled or creped
    • Y10T428/24455—Paper
    • Y10T428/24463—Plural paper components
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24479—Structurally defined web or sheet [e.g., overall dimension, etc.] including variation in thickness
    • Y10T428/24612—Composite web or sheet
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24628—Nonplanar uniform thickness material
    • Y10T428/24736—Ornamental design or indicia

Definitions

  • the invention relates to the field of absorbent papers, wadding cellulose, for household use.
  • a complex sheet composed of two folds of absorbent paper of cellulose wadding of the conventional crepe type, whose grammage is between 10 and 40 g / cm 2 and which are embossed by calendering according to fine patterns comprising protuberances, and which are linked together, in particular by gluing, at the level of the surfaces of the vertices of the coincident protuberances of said two folds.
  • US 3,414,459 describes a process for embossing and bonding two plies together cellulose wadding, using the so-called point-to-point technique.
  • the two plies are embossed separately by means of identical metal cylinders which are provided with pins and which cooperate respectively with coated rollers made of rubber.
  • This technique requires that the two cylinders have symmetrical patterns and that the pins of the two cylinders coincide perfectly in the tightening interval. A radial or circumferential offset between the pins of the two cylinders can cause absence of connection in certain areas of the complex sheet obtained.
  • US 5,173,351 has proposed using patterns with different pitch in at least one direction on the two embossing cylinders so ensure at least one connection point on the elementary complex sheets obtained by cutting the complex sheet leaving the installation.
  • WO 96/32248 proposes to link only certain areas of the two folds embossed by applying the glue only on the ends of the protrusions of one of the folds, which must participate in the effective connection.
  • the two cylinders must have symmetrical patterns and the pins of the two cylinders must coincide precisely at the tightening interval.
  • the pins are arranged on the cylinders on generators, large circles and propellers regularly spaced.
  • the protrusions formed on the folds by the imprint of the pins are aligned in preferred directions and with spacings constant.
  • the observer who looks at the outside faces of the complex sheet has the impression that these faces include geometric designs including only straight lines or line segments.
  • the object of the invention is to improve the absorption as well as the flexibility of complex sheets defined above while ensuring that the end product keeps the same aspect as that obtained by current techniques and to ensure that we can overcome the constraints imposed in the choice of patterns and in the precise setting of the embossing cylinders.
  • the total bonded area of the vertices of the protrusions of a fold is at least equal to 20% of the surfaces of the vertices of the protrusions of said fold.
  • the surface of the vertices of the protrusions of each fold is less than 30% of the total area of said fold. This surface is preferably greater than 7.5% of the total area of the fold, and preferably less than 15% of the fold surface.
  • the density of the protrusions of each ply is less than 30 protuberances per square centimeter and preferably less than 20.
  • the two folds are embossed according to artistic patterns, the two patterns which may or may not be identical.
  • An offset of the two patterns between them can be achieved by a translation or by rotating the imprint of the pattern of an embossing cylinder relative to the imprint of the pattern on the other cylinder.
  • FIGS. 1a to 1d show examples of embossing patterns provided on the embossing rolls of an installation for manufacturing a complex sheet composed of two plies of absorbent paper of cellulose wadding, of the conventional creped type, (of CWP type), and whose grammage is between 10 and 40 g / cm 2 .
  • a complex sheet composed of two plies of absorbent paper of cellulose wadding, of the conventional creped type, (of CWP type), and whose grammage is between 10 and 40 g / cm 2 .
  • Such a sheet is used for domestic use as household paper or "paper towel”.
  • the patterns have artistic looks, as opposed to the usual geometric patterns, that is to say, in a pattern, the distances between any spike of neighboring pins are varied and the directions between any pin and the adjacent pins are also varied.
  • the pins of a pattern seem to be arranged on curved lines, or concentric circles.
  • the protrusions formed by embossing on the folds are also arranged on one side of the fold according to the same patterns.
  • the two folds to form a complex sheet can be embossed with identical patterns or with different patterns.
  • the two folds are connected together, by the technique known as point against point, but with an offset of two patterns in one direction.
  • the non-coincident protuberances are arranged, between coincident protuberances, a bit like what you get with the technique that allows you to get a structure called "nested". These protrusions are not related to the other fold and create pockets.
  • the product obtained is also more flexible and more pleasant to the touch. because of the reduction in the number of connection points. Correlatively, the rigidity of the product and its resistance to dry or wet rupture are slightly reduced. However, it was found that this loss of resistance was less than the gain in absorption. As the main function of a “paper towel” is to absorb liquids, we can easily define a product with a combination optimal absorption / resistance.
  • the density of the pins must be greater than 10 pins and less than 30 per cm 2 and preferably between 15 and 20 pins per cm 2 .
  • the surface of the peaks of the pins, and by the same token, the surface of the peaks protuberances is greater than 5%, and preferably less than 30% of the total surface.
  • the pattern designs are chosen so that 25% of protrusions of each fold, and preferably 30%, or even up to 70%, participate in effective connections of the two folds.
  • the total of the surfaces linked at the level of the protrusions participating in the connections effective represents at least 15% and advantageously 20% of the surface total of the vertices of each fold.
  • Measurements made it possible to count the connection points for different types of patterns. These measurements are carried out by image analysis. We determine at using a camera the gray value generated by the imprint left on a paper carbon by the connection points with respect to a reference value without point, then we apply a coefficient according to the average surface occupied by a single point.
  • the dark gray threshold of the areas of effective contact between protrusions, areas of the image at this threshold or darker are colored black, the rest are colored white.
  • the image can then be transformed into a binary image (black and white) more contrasted as the initial image in gray level.
  • This is done using graphics software such as Photoscop (ADOBE) or Picture Publisher (MICOGRAFX).
  • Photoscop ADOBE
  • MICOGRAFX Picture Publisher
  • FIGS. 2a to 2d show the distributions of the connection points for complex sheets with embossed folds with identical and offset patterns corresponding respectively to the patterns shown in Figures 1a to 2d.
  • Figure 2e shows the distribution of the connection points of a complex sheet one of the folds includes the pattern shown in Figure 1b and the other fold has the pattern shown in Figure 1c.
  • the maximum contact surface i.e. 1.18 mm 2
  • the surface at the top of the pins which is 0.8 mm 2 , since there is undoubtedly some crushing during application glue on the tops of the protrusions of a fold, or when applying the first fold to the second fold in between the two embossing rolls, or even when creating rolls of complex sheet at the exit of the installation for making this complex sheet.
  • the installation for producing the complex sheet according to the invention is known in itself and of the type used to make connections of two point-to-point folds.
  • the offset of the patterns between the two folds can be achieved in a direction preferential, in general the direction of advancement of the sheet, by angularly shifting one of the embossing cylinders relative to the other.
  • the offset can also be obtained by pivoting one pattern with respect to the other. This can be obtained during the machining of the two embossing cylinders.
  • samples A to E and samples A ', B', C ', D' correspond to the same patterns 1a to 1d but assembled in perfect position points against points.
  • the absorption was measured according to the AFNOR NF Q03-068 method. This method consists of immersing a test tube in water and then determining the mass of water absorbed after a draining time under specified conditions.
  • the graphs represented in FIGS. 3 and 4 have been drawn by plotting the measured values of the absorption, expressed in cm 3 per gram of sample, and on the abscissa the measured values of wet resistances crosswise for different embossing pressures. These values are expressed in N / m.
  • the graphs show that the performances of products A to E are superior to those of products A ', D' respectively for the same values of wet resistance crosswise.
  • embossed samples were made from the same CWP tissue paper according to a pattern, the elementary pattern of which comprises three diamonds nested together and whose density of the protuberances is 6 protuberances per cm 2 .
  • the first series of samples Lp is of the point against point type
  • the second series Ld is offset from the patterns with 20% of bond density. It can be seen that the offset does not bring any improvement in absorption.

Abstract

The domestic two-ply absorbent paper material, with an embossed patterning and in a weight of 10-40 g/m<2>, has a raised point density in each ply of ≥ 10 points/cm<2>, and the surface area of the raised points in each ply is ≥ 5% of the ply surface. At least one ply is embossed with a decorative pattern, with structured projection gaps and angles, which match up with the embossed projections of the other ply. The total surface of the peaks of the projections, bonded together, are at least 15% of the total projection peak surface area of the ply, at the relative positions for the pattern of the two plys. At least 30% or 40% of the embossed projections of one ply form bonds with the embossed projections of the other ply. The total surface of the projection peaks, in a ply, is at least equal to 20% of the projection surfaces of the ply, and is ≤ 30% of the ply surface area and ≥ 7.5% of the ply surface while ≤ 15%. The projection density is preferably ≤ 20 projections/cm<2>. Both plys are embossed with a decorative pattern which can be identical and offset, or different.

Description

L'invention se rapporte au domaine des papiers absorbants, en ouate de cellulose, à usage domestique.The invention relates to the field of absorbent papers, wadding cellulose, for household use.

Elle concerne plus précisément une feuille complexe composée de deux plis de papier absorbant en ouate de cellulose du type crêpé conventionnel, dont le grammage est compris entre 10 et 40 g/cm2 et qui sont gaufrés par calandrage selon des motifs fins comportant des protubérances, et qui sont liés entre eux, notamment par collage, au niveau des surfaces des sommets des protubérances coïncidentes desdits deux plis.More precisely, it relates to a complex sheet composed of two folds of absorbent paper of cellulose wadding of the conventional crepe type, whose grammage is between 10 and 40 g / cm 2 and which are embossed by calendering according to fine patterns comprising protuberances, and which are linked together, in particular by gluing, at the level of the surfaces of the vertices of the coincident protuberances of said two folds.

US 3 414 459 décrit un procédé pour gaufrer et lier entre eux deux plis en ouate de cellulose, selon la technique dite pointes contre pointes. Selon cette technique on gaufre les deux plis séparément au moyen de cylindres métalliques identiques qui sont munis de picots et qui coopèrent respectivement avec des rouleaux à revêtement en caoutchouc. On enduit ensuite les sommets des protubérances sur l'un des plis d'une colle appropriée. On lie enfin les deux plis l'un à l'autre par les sommets des protubérances par serrage entre les deux cylindres gaufreurs calés en rotation l'un par rapport à l'autre de façon que les picots viennent pointes contre pointes. Cette technique exige que les deux cylindres comportent des motifs symétriques et que les picots des deux cylindres coïncident parfaitement dans l'intervalle de serrage. Un décalage radial ou circonférentiel entre les picots des deux cylindres peut entraíner une absence de liaison dans certaines zones de la feuille complexe obtenue.US 3,414,459 describes a process for embossing and bonding two plies together cellulose wadding, using the so-called point-to-point technique. According to this technique the two plies are embossed separately by means of identical metal cylinders which are provided with pins and which cooperate respectively with coated rollers made of rubber. We then coat the tops of the protrusions on one of the folds an appropriate glue. Finally, we link the two folds to each other by the tops of the protrusions by clamping between the two embossing cylinders, which are set in rotation one by relative to each other so that the pins come points against points. This technique requires that the two cylinders have symmetrical patterns and that the pins of the two cylinders coincide perfectly in the tightening interval. A radial or circumferential offset between the pins of the two cylinders can cause absence of connection in certain areas of the complex sheet obtained.

Pour remédier à cet inconvénient, US 5 173 351 a proposé d'utiliser des motifs à pas différents dans au moins une direction sur les deux cylindres gaufreurs afin d'assurer au moins un point de liaison sur les feuilles complexes élémentaires obtenues par découpe de la feuille complexe sortant de l'installation.To remedy this drawback, US 5,173,351 has proposed using patterns with different pitch in at least one direction on the two embossing cylinders so ensure at least one connection point on the elementary complex sheets obtained by cutting the complex sheet leaving the installation.

Enfin, WO 96/32248 propose de ne lier que certaines zones des deux plis gaufrés en n'appliquant la colle que sur les extrémités des protubérances de l'un des plis, qui doivent participer à la liaison effective. Ici aussi, les deux cylindres doivent comporter des motifs symétriques et les picots des deux cylindres doivent coïncider avec précision au niveau de l'intervalle de serrage.Finally, WO 96/32248 proposes to link only certain areas of the two folds embossed by applying the glue only on the ends of the protrusions of one of the folds, which must participate in the effective connection. Here too, the two cylinders must have symmetrical patterns and the pins of the two cylinders must coincide precisely at the tightening interval.

Dans ces trois documents, il est prévu que les picots sont disposés sur les cylindres selon des génératrices, des grands cercles et des hélices régulièrement espacés. Il en résulte que les protubérances formées sur les plis par l'empreinte des picots sont alignées dans des directions préférentielles et avec des écartements constants. L'observateur qui regarde les faces extérieures de la feuille complexe a l'impression que ces faces comportent des dessins géométriques comportant uniquement des lignes droites ou des segments de droite.In these three documents, it is provided that the pins are arranged on the cylinders on generators, large circles and propellers regularly spaced. As a result, the protrusions formed on the folds by the imprint of the pins are aligned in preferred directions and with spacings constant. The observer who looks at the outside faces of the complex sheet has the impression that these faces include geometric designs including only straight lines or line segments.

On conçoit qu'un léger décalage axial ou circonférentiel entre les deux cylindres gaufreurs par suite du manque de synchronisme ou de l'usure des pièces d'entraínement puisse provoquer une absence de coïncidence entre les picots au niveau de l'intervalle de serrage des cylindres gaufreurs et entraíner des rebuts de fabrication.We can see that a slight axial or circumferential offset between the two embossing cylinders due to lack of synchronism or wear of parts drive could cause an absence of coincidence between the pins at the level of the clamping interval of the embossing rolls and cause manufacturing waste.

D'autres techniques d'assemblage des plis permettent d'emboíter les protubérances de l'un des plis entre les protubérances de l'autre pli afin d'obtenir une structure dénommée « nested » qui entraíne un degré d'absorption amélioré. Avec cette technique, les cylindres gaufreurs sont écartés l'un de l'autre et on retire le pli gaufré de l'un des cylindres pour l'emboíter dans l'autre pli en le passant dans un intervalle de serrage ménagé entre l'autre cylindre gaufreur et un cylindre complémentaire lisse. Cette technique exige également un parfait synchronisme entre les deux cylindres gaufreurs.Other ply assembly techniques make it possible to nest the protrusions of one of the folds between the protrusions of the other fold in order to obtain a structure called "nested" which results in an improved degree of absorption. With this technique, the embossing cylinders are spaced from each other and the fold is removed embossed from one of the cylinders to nest it in the other fold by passing it through a tightening interval between the other embossing cylinder and a cylinder complementary smooth. This technique also requires perfect synchronism between the two embossing cylinders.

Le but de l'invention est d'améliorer l'absorption ainsi que la souplesse des feuilles complexes définies ci-dessus tout en faisant en sorte que le produit final garde le même aspect que celui obtenu par les techniques actuelles et de faire en sorte que l'on puisse s'affranchir des contraintes imposées dans le choix des motifs et dans le calage précis des cylindres gaufreurs.The object of the invention is to improve the absorption as well as the flexibility of complex sheets defined above while ensuring that the end product keeps the same aspect as that obtained by current techniques and to ensure that we can overcome the constraints imposed in the choice of patterns and in the precise setting of the embossing cylinders.

L'invention atteint son but par le fait que :

  • a) la densité des protubérances de chaque pli est supérieure à 10 protubérances par cm2 et la surface des sommets des protubérances de chaque pli est supérieure à 5 % de la surface dudit pli ;
  • b) on gaufre au moins l'un des plis selon un motif artistique dans lequel les distances et les directions de n'importe quelle protubérance avec les protubérances adjacentes sont variées, ledit motif étant choisi de telle manière qu'au moins 25 % des protubérances dudit pli participent à des liaisons effectives avec des protubérances coïncidentes de l'autre pli, et que la surface totale liée des sommets des protubérances dudit plis qui participent aux liaisons représente au moins 15 % de la surface totale des sommets des protubérances dudit pli, quelle que soit la position relative des motifs des deux plis.
    • The invention achieves its object by the fact that:
  • a) the density of the protuberances of each ply is greater than 10 protrusions per cm 2 and the area of the apexes of the protrusions of each ply is greater than 5% of the surface of said ply;
  • b) at least one of the folds is embossed according to an artistic motif in which the distances and directions of any protuberance with the adjacent protuberances are varied, said motif being chosen so that at least 25% of the protuberances of said fold participate in effective connections with coincident protuberances of the other fold, and that the total bound surface of the vertices of the protrusions of said folds which participate in the connections represents at least 15% of the total surface of the vertices of the protuberances of said fold whatever the relative position of the patterns of the two folds.

    • Avantageusement, 30 % et encore plus avantageusement 40 % des protubérances d'un pli participent à des liaisons effectives avec les protubérances coïncidentes de l'autre pli. On a constaté que jusqu'à 70 % on avait encore une amélioration.Advantageously, 30% and even more advantageously 40% of protrusions of a fold participate in effective connections with the protrusions coincide with the other fold. We found that up to 70% we still had improvement.

    De préférence, la surface totale liée des sommets des protubérances d'un pli est au moins égale à 20 % des surfaces des sommets des protubérances dudit pli.Preferably, the total bonded area of the vertices of the protrusions of a fold is at least equal to 20% of the surfaces of the vertices of the protrusions of said fold.

    De manière avantageuse, la surface des sommets des protubérances de chaque pli est inférieure à 30 % de la surface totale dudit pli. Cette surface est de préférence supérieure à 7,5 % de la surface totale du pli, et de préférence inférieure à 15 % de la surface du pli. La densité des protubérances de chaque pli est inférieure à 30 protubérances par centimètre carré et de préférence inférieure à 20. Advantageously, the surface of the vertices of the protrusions of each fold is less than 30% of the total area of said fold. This surface is preferably greater than 7.5% of the total area of the fold, and preferably less than 15% of the fold surface. The density of the protrusions of each ply is less than 30 protuberances per square centimeter and preferably less than 20.

    Avantageusement, les deux plis sont gaufrés selon des motifs artistiques, les deux motifs pouvant être identiques ou non.Advantageously, the two folds are embossed according to artistic patterns, the two patterns which may or may not be identical.

    Un décalage des deux motifs entre eux peut être réalisé par une translation ou par une rotation de l'empreinte du motif d'un cylindre gaufreur par rapport à l'empreinte du motif de l'autre cylindre.An offset of the two patterns between them can be achieved by a translation or by rotating the imprint of the pattern of an embossing cylinder relative to the imprint of the pattern on the other cylinder.

    D'autres caractéristiques et avantages de l'invention ressortiront à la lecture de la description suivante faite à titre d'exemple et en référence aux dessins annexés dans lesquels :

    • les figures 1a à 1d montrent quatre motifs artistiques formés par des picots de cylindres gaufreurs afin de réaliser des protubérances sur les plis constitutifs d'une feuille complexe ;
    • les figures 2a et 2e montrent les traces des liaisons entre les surfaces des sommets des protubérances des deux plis formées respectivement par des motifs de picots représentés sur les figures 1a à 1d, et par une combinaison des motifs des figures 1b et 1c.
    • les figures 3 et 4 sont des graphiques représentent pour différents motifs la variation de l'absorption, exprimée en cm3 par gramme de papier, en fonction de la résistance humide du produit mesurée sens travers, exprimée en N/m
    Other characteristics and advantages of the invention will emerge on reading the following description given by way of example and with reference to the appended drawings in which:
    • Figures 1a to 1d show four artistic patterns formed by spikes of embossing cylinders in order to produce protuberances on the folds constituting a complex sheet;
    • FIGS. 2a and 2e show the traces of the connections between the surfaces of the vertices of the protuberances of the two plies formed respectively by patterns of spikes represented in FIGS. 1a to 1d, and by a combination of the patterns in FIGS. 1b and 1c.
    • Figures 3 and 4 are graphs represent for different reasons the variation in absorption, expressed in cm3 per gram of paper, as a function of the wet resistance of the product measured crosswise, expressed in N / m

    On a représenté sur les figures 1a à 1d des exemples de motifs de gaufrage prévus sur les cylindres gaufreurs d'une installation de fabrication d'une feuille complexe composée de deux plis de papier absorbant en ouate de cellulose, du type conventionnel crêpé, (du type CWP), et dont le grammage est compris entre 10 et 40 g/cm2. On utilise une telle feuille en usage domestique en tant papier de ménage ou « essuie-tout ».FIGS. 1a to 1d show examples of embossing patterns provided on the embossing rolls of an installation for manufacturing a complex sheet composed of two plies of absorbent paper of cellulose wadding, of the conventional creped type, (of CWP type), and whose grammage is between 10 and 40 g / cm 2 . Such a sheet is used for domestic use as household paper or "paper towel".

    Les points dessinés sur ces figures 1a et 1d représentent les extrémités de picots prévus sur les cylindres gaufreurs pour former des protubérances sur les plis par déformation mécanique du pli qui passe dans un intervalle de gaufrage ménagé entre le cylindre gaufreur et un cylindre en caoutchouc associé d'axe parallèle au cylindre gaufreur.The points drawn in these figures 1a and 1d represent the ends of pins provided on the embossing cylinders to form protuberances on the pleats by mechanical deformation of the fold which passes through an embossing interval formed between the embossing cylinder and an associated rubber cylinder with an axis parallel to the cylinder embosser.

    Ainsi qu'on le voit sur les figures 1a à 1d, les motifs ont des allures artistiques, par opposition aux motifs géométriques habituels, c'est-à-dire que, dans un motif, les distances séparant un picot quelconque de picots voisins sont variées et les directions entre un picot quelconque et les picots adjacents sont également variées. Pour l'observateur, les picots d'un motif semblent être disposés sur des lignes courbes, ou des cercles concentriques.As can be seen in FIGS. 1a to 1d, the patterns have artistic looks, as opposed to the usual geometric patterns, that is to say, in a pattern, the distances between any spike of neighboring pins are varied and the directions between any pin and the adjacent pins are also varied. For the observer, the pins of a pattern seem to be arranged on curved lines, or concentric circles.

    Les protubérances formées par gaufrage sur les plis sont également disposées sur une face du pli selon les mêmes motifs.The protrusions formed by embossing on the folds are also arranged on one side of the fold according to the same patterns.

    Les deux plis devant constituer une feuille complexe peuvent être gaufrés avec des motifs identiques ou avec des motifs différents. The two folds to form a complex sheet can be embossed with identical patterns or with different patterns.

    Lorsque les deux motifs sont identiques, les deux plis sont reliés entre eux, par la technique connue sous le nom de pointes contre pointes, mais avec un décalage des deux motifs dans une direction. De cette manière seules quelques protubérances de l'un des plis coïncident avec des protubérances de l'autre pli et sont liées à elles. Les protubérances non coïncidentes sont disposées, entre des protubérances coïncidentes, un peu à la manière de ce que l'on obtient avec la technique qui permet d'obtenir une structure dénommée « nested ». Ces protubérances ne sont pas liées à l'autre pli et créent des poches. La présence de ces protubérances non liées par les poches ainsi formées permet d'améliorer l'absorption du produit final par rapport au même produit dans lequel les deux plis ont les mêmes motifs et sont réunis pointes contre pointes ,sans décalage, c'est à dire de telle manière que toutes les protubérances d'un pli coïncident et sont liées aux protubérances de l'autre pli.When the two patterns are identical, the two folds are connected together, by the technique known as point against point, but with an offset of two patterns in one direction. In this way only a few protrusions of one of the folds coincides with protrusions of the other fold and are linked to them. The non-coincident protuberances are arranged, between coincident protuberances, a bit like what you get with the technique that allows you to get a structure called "nested". These protrusions are not related to the other fold and create pockets. The presence of these protrusions not bound by the pockets as well formed improves the absorption of the final product compared to the same product in which the two folds have the same patterns and are joined points against points , without offset, that is to say in such a way that all the protuberances of a fold coincide and are related to the protrusions of the other fold.

    Le produit obtenu est également plus souple et plus agréable au toucher en raison de la réduction du nombre de points de liaison. Corrélativement, la rigidité du produit et sa résistance à la rupture sèche ou humide sont légèrement diminuées. Cependant on a constaté que cette perte de résistance était inférieure au gain en absorption. Comme la fonction principale d'un « essuie-tout » est d'absorber les liquides, on peut aisément définir un produit présentant une combinaison absorption/résistance optimale.The product obtained is also more flexible and more pleasant to the touch. because of the reduction in the number of connection points. Correlatively, the rigidity of the product and its resistance to dry or wet rupture are slightly reduced. However, it was found that this loss of resistance was less than the gain in absorption. As the main function of a “paper towel” is to absorb liquids, we can easily define a product with a combination optimal absorption / resistance.

    Du fait de la disposition des protubérances selon des motifs artistiques, on est assuré que plusieurs d'entre elles seront coïncidentes lorsque les motifs des deux plis sont décalés, alors que, dans les structures du type pointes pointes actuelles dans lesquelles les motifs ont des dessins géométriques formés de segments de droite dans des directions privilégiées, un décalage minime entre les motifs des deux plis entraíne une absence de liaison dans certaines zones de la feuille complexe.Due to the arrangement of the protuberances on artistic grounds, we are assured that several of them will be coincident when the patterns of the two folds are shifted, whereas, in the structures of the point type points current in which the patterns have geometric designs formed of line segments in privileged directions, a minimal offset between the patterns of the two folds results an absence of connection in certain areas of the complex sheet.

    Pour qu'il se produise des coïncidences certaines dans une proportion suffisante pour assurer la liaison des deux plis, certaines conditions doivent être respectées.In order for certain coincidences to occur in a proportion sufficient to ensure the connection of the two folds, certain conditions must be respected.

    La densité des picots doit être supérieure à 10 picots et inférieure à 30 par cm2 et de préférence entre 15 et 20 picots par cm2.The density of the pins must be greater than 10 pins and less than 30 per cm 2 and preferably between 15 and 20 pins per cm 2 .

    La surface des sommets des picots, et par le fait même, la surface des sommets des protubérances est supérieure à 5 %, et de préférence inférieure à 30 % de la surface totale.The surface of the peaks of the pins, and by the same token, the surface of the peaks protuberances is greater than 5%, and preferably less than 30% of the total surface.

    Les dessins des motifs sont choisis de telle manière que 25 % des protubérances de chaque pli, et de préférence 30 %, voire jusqu'à 70 %, participent à des liaisons effectives des deux plis.The pattern designs are chosen so that 25% of protrusions of each fold, and preferably 30%, or even up to 70%, participate in effective connections of the two folds.

    Le total des surfaces liées au niveau des protubérances participant aux liaisons effectives représente au moins 15 % et de manière avantageuse 20 % de la surface totale des sommets de chaque pli. The total of the surfaces linked at the level of the protrusions participating in the connections effective represents at least 15% and advantageously 20% of the surface total of the vertices of each fold.

    Des mesures ont permis de dénombrer les points de liaison pour différents types de motifs. Ces mesures sont réalisées par analyse d'images. On détermine au moyen d'une caméra la valeur de gris engendrée par l'empreinte laissée sur un papier carbone par les points de liaison par rapport à une valeur de référence sans point, puis on applique un coefficient en fonction de la surface moyenne occupée par un seul point.Measurements made it possible to count the connection points for different types of patterns. These measurements are carried out by image analysis. We determine at using a camera the gray value generated by the imprint left on a paper carbon by the connection points with respect to a reference value without point, then we apply a coefficient according to the average surface occupied by a single point.

    Pour cela, dans une première étape, on numérise au scanner le calque d'empreinte en niveaux de gris à 300 points par pouce.For this, in a first step, we scan the layer with a scanner grayscale footprint at 300 dots per inch.

    Dans une deuxième étape, on détermine le seuil de gris foncé des zones de contact effectif entre protubérances, les zones de l'image à ce seuil ou plus foncées sont colorées en noir, le reste est coloré en blanc.In a second step, the dark gray threshold of the areas of effective contact between protrusions, areas of the image at this threshold or darker are colored black, the rest are colored white.

    L'image peut alors être transformée en image binaire (noir et blanc) plus contrastée que l'image de départ en niveau de gris. Cette opération se fait à l'aide de logiciels graphiques tels que Photoscop (ADOBE) ou Picture Publisher (MICOGRAFX). A ce stade, il est possible de mesurer le pourcentage de la surface noire représentant les zones de liaison à l'aide de ces mêmes logiciels.The image can then be transformed into a binary image (black and white) more contrasted as the initial image in gray level. This is done using graphics software such as Photoscop (ADOBE) or Picture Publisher (MICOGRAFX). At this point, it is possible to measure the percentage of the area black representing the connection areas using the same software.

    Si l'on désire plus d'informations sur cette image, il est possible dans une troisième étape de reprendre l'image par un analyseur d'image tel que le Quantiniet 600 (LECA) qui en plus du pourcentage de surface liée peut calculer le nombre de points par cm2, la surface de ces points ainsi que leur répartition sur un histogramme.If you want more information on this image, it is possible in a third step to take the image by an image analyzer such as the Quantiniet 600 (LECA) which in addition to the percentage of bound surface can calculate the number of points per cm 2 , the area of these points as well as their distribution on a histogram.

    Les figures 2a à 2d montrent les répartitions des points de liaison pour des feuilles complexes comportant de plis gaufrés avec des motifs identiques et décalés correspondant respectivement aux motifs représentés sur les figures 1a à 2d.FIGS. 2a to 2d show the distributions of the connection points for complex sheets with embossed folds with identical and offset patterns corresponding respectively to the patterns shown in Figures 1a to 2d.

    La figure 2e montre la répartition des points de liaison d'une feuille complexe dont l'un des plis comporte le motif montré sur la figure 1b et l'autre pli comporte le motif représenté sur la figure 1c.Figure 2e shows the distribution of the connection points of a complex sheet one of the folds includes the pattern shown in Figure 1b and the other fold has the pattern shown in Figure 1c.

    Le tableau suivant montre les valeurs comparatives de cinq échantillons référencés A et E, les références A à C correspondent à des feuilles complexes ayant des motifs identiques correspondant respectivement aux figures 1a à 1c, et la référence D correspondant à un échantillon dont l'un des plis comporte le motif de la figure 1b et l'autre pli le motif de la figure 1c.

    • la colonne C1 indique le nombre de protubérances par cm2,
    • la colonne C2 indique le nombre de liaisons effectives par cm2,
    • la colonne C3 est le rapport en % entre les valeurs des colonnes C2 et C1,
    • la colonne C4 indique le pourcentage de la surface des sommets des protubérances par rapport à la surface totale. Elle correspond à la surface associée en véritables pointes pointes,
    • la colonne C5 représente le pourcentage de la surface liée des sommets par rapport à la surface totale, et
    • la colonne C6 est le rapport en % entre les valeurs des colonnes C5 et C4. C1 C2 C3 % C4 % C5 % C6 % A 15,7 10,5 66 12,3 4,5 37 B 15,2 7,7 50 9,6 2,2 23 C 15,4 7 45 9,8 2 20 D 12 7,2 60 7,6 2,7 35 E (B + C) 15,3 6,8 44 9,7 1,9 20
    The following table shows the comparative values of five samples referenced A and E, the references A to C correspond to complex sheets having identical patterns corresponding respectively to FIGS. 1a to 1c, and the reference D corresponding to a sample of which one of the folds include the pattern in Figure 1b and the other fold the pattern in Figure 1c.
    • column C1 indicates the number of protrusions per cm 2 ,
    • column C2 indicates the number of effective connections per cm 2 ,
    • column C3 is the ratio in% between the values of columns C2 and C1,
    • column C4 indicates the percentage of the surface of the vertices of the protrusions in relation to the total surface. It corresponds to the surface associated in real points,
    • column C5 represents the percentage of the bounded area of the vertices in relation to the total area, and
    • column C6 is the ratio in% between the values of columns C5 and C4. C1 C2 C3% C4% C5% C6% AT 15.7 10.5 66 12.3 4.5 37 B 15.2 7.7 50 9.6 2.2 23 VS 15.4 7 45 9.8 2 20 D 12 7.2 60 7.6 2.7 35 E (B + C) 15.3 6.8 44 9.7 1.9 20

    Avec un autre échantillon référencé A, mais un décalage différent, on a obtenu une surface liée correspondant à 3,3 % de la surface totale de la feuille soit 7.8 liaisons effectives par cm2.With another sample referenced A, but with a different offset, a bonded surface corresponding to 3.3% of the total surface of the sheet was obtained, ie 7.8 effective bonds per cm 2 .

    Les mesures des surfaces et des points de liaison, c'est-à-dire les surfaces de contact collées entre les protubérances coïncidentes ont donné les valeurs suivantes : Surface moyenne des points de liaison 0,42 mm2 Surface de contact maximale 1,18 mm2 Surface de contact minimale 0,12 mm2 The measurements of the surfaces and the connection points, that is to say the contact surfaces glued between the coincident protuberances, gave the following values: Average surface of the connection points 0.42 mm 2 Maximum contact area 1.18 mm 2 Minimum contact area 0.12 mm 2

    Il a été constaté que la surface de contact maximale (soit 1,18 mm2) est supérieure à la surface au sommet des picots qui est de 0,8 mm2, car il y a sans doute un certain écrasement lors de l'application de la colle sur les sommets des protubérances d'un pli, ou lors de l'application du premier pli sur le deuxième pli dans l'intervalle des deux cylindres gaufreurs, ou même lors de la création de rouleaux de feuille complexe à la sortie de l'installation permettant de réaliser cette feuille complexe.It has been found that the maximum contact surface (i.e. 1.18 mm 2 ) is greater than the surface at the top of the pins which is 0.8 mm 2 , since there is undoubtedly some crushing during application glue on the tops of the protrusions of a fold, or when applying the first fold to the second fold in between the two embossing rolls, or even when creating rolls of complex sheet at the exit of the installation for making this complex sheet.

    L'installation pour réaliser la feuille complexe selon l'invention est connue en soi et du type de celle utilisée pour faire de liaisons de deux plis pointes contre pointes.The installation for producing the complex sheet according to the invention is known in itself and of the type used to make connections of two point-to-point folds.

    Le décalage des motifs entre les deux plis peut être réalisé selon une direction préférentielle, en général le sens d'avancement de la feuille, en décalant angulairement l'un des cylindres gaufreurs par rapport à l'autre. Le décalage peut être également obtenu par pivotement d'un motif par rapport à l'autre. Ceci peut être obtenu lors de l'usinage des deux cylindres gaufreurs.The offset of the patterns between the two folds can be achieved in a direction preferential, in general the direction of advancement of the sheet, by angularly shifting one of the embossing cylinders relative to the other. The offset can also be obtained by pivoting one pattern with respect to the other. This can be obtained during the machining of the two embossing cylinders.

    ESSAISTESTS

    A partir d'un même papier tissue crêpé, 100% kraft de résineux, on a réalisé des échantillons de produits selon les motifs représentés sur les figures 1a à 1d pour différentes pressions de gaufrage. En effet, en augmentant la pression de gaufrage pour un même motif, on améliore la capacité d'absorption mais on réduit corrélativement la résistance à la rupture. Afin de pouvoir comparer les propriétés des échantillons il est donc nécessaire de tenir compte de la perte de résistance induite, en particulier de la résistance humide sens travers qui est un paramètre important pour caractériser les essuie-toutFrom the same creped tissue paper, 100% softwood kraft, we produced product samples according to the patterns shown in Figures 1a to 1d for different embossing pressures. Indeed, by increasing the embossing pressure for the same reason, the absorption capacity is improved but the correlation is reduced Tear resistant. In order to be able to compare the properties of the samples it is therefore necessary to take into account the loss of resistance induced, in particular the wet resistance crosswise which is an important parameter to characterize paper towels

    Afin de montrer l'amélioration apportée par la solution de l'invention, on a réalisé les échantillons A à E et des échantillons A', B', C', D'. Ces derniers correspondent aux mêmes motifs 1a à 1d mais assemblés en position parfaitement pointes contre pointes.In order to show the improvement brought by the solution of the invention, we have samples A to E and samples A ', B', C ', D'. These latter correspond to the same patterns 1a to 1d but assembled in perfect position points against points.

    On a mesuré l'absorption selon la méthode AFNOR NF Q03-068. Cette méthode consiste à immerger une éprouvette dans l'eau puis à déterminer la masse d'eau absorbée après un temps d'égouttage dans des conditions spécifiées. On a tracé les graphes représentés sur les figures 3 et 4 en reportant en ordonnées les valeurs mesurées de l'absorption, exprimées en cm3 par gramme d'échantillon et en abscisses les valeurs mesurées de résistances humides sens travers pour différentes pressions de gaufrage. Ces valeurs sont exprimées en N/m.
    Les graphes montrent que les performances des produits A à E sont supérieures à celles des produits A', D' respectivement pour les mêmes valeurs de résistance humide sens travers.    The absorption was measured according to the AFNOR NF Q03-068 method. This method consists of immersing a test tube in water and then determining the mass of water absorbed after a draining time under specified conditions. The graphs represented in FIGS. 3 and 4 have been drawn by plotting the measured values of the absorption, expressed in cm 3 per gram of sample, and on the abscissa the measured values of wet resistances crosswise for different embossing pressures. These values are expressed in N / m.
    The graphs show that the performances of products A to E are superior to those of products A ', D' respectively for the same values of wet resistance crosswise.

    A titre de contre-exemple, on a réalisé à partir du même papier tissue CWP des échantillons gaufrés selon un motif dont le motif élémentaire comprend trois losanges imbriqués entre eux et dont la densité des protubérances est de 6 protubérances par cm2. La première série d'échantillons Lp est du type pointes contre pointes, la seconde série Ld est à décalage des motifs avec 20% de densité de liaison. On constate que le décalage n'apporte aucune amélioration de l'absorption.As a counterexample, embossed samples were made from the same CWP tissue paper according to a pattern, the elementary pattern of which comprises three diamonds nested together and whose density of the protuberances is 6 protuberances per cm 2 . The first series of samples Lp is of the point against point type, the second series Ld is offset from the patterns with 20% of bond density. It can be seen that the offset does not bring any improvement in absorption.

    Claims (11)

    Feuille complexe composée d'au moins deux plis de papier absorbant en ouate de cellulose du type conventionnel à pressage en partie humide, dont le grammage est compris entre 10 et 40 g/m2, qui sont gaufrés par calandrage selon des motifs fins comportant des protubérances, et qui sont liés entre eux, notamment par collage, au niveau des surfaces des sommets des protubérances coïncidentes desdits deux plis, caractérisée par le fait que : a) la densité des protubérances de chaque pli est supérieure à 10 protubérances par cm2 et la surface des sommets des protubérances de chaque pli est supérieure à 5 % de la surface totale dudit pli ; b) au moins l'un des plis est gaufré selon un motif artistique dans lequel les distances et les directions de n'importe quelle protubérance avec les protubérances adjacentes sont variées, ledit motif étant choisi de telle manière qu'au moins 25 % des protubérances dudit pli participent à des liaisons effectives avec des protubérances coïncidentes de l'autre pli, et que la surface totale des sommets des protubérances dudit plis qui participent aux liaisons représente au moins 15 % de la surface totale des sommets des protubérances dudit pli, quelle que soit la position relative des motifs des deux plis. Complex sheet composed of at least two plies of absorbent paper of cellulose wadding of the conventional type with a wet pressing, the grammage of which is between 10 and 40 g / m 2 , which are embossed by calendering according to fine patterns comprising protrusions, and which are linked together, in particular by gluing, at the level of the surfaces of the vertices of the coincident protuberances of said two plies, characterized in that: a) the density of the protrusions of each ply is greater than 10 protrusions per cm 2 and the area of the apexes of the protrusions of each ply is greater than 5% of the total area of said ply; b) at least one of the folds is embossed according to an artistic motif in which the distances and directions of any protuberance with the adjacent protuberances are varied, said motif being chosen so that at least 25% of the protuberances of said fold participate in effective connections with coincident protuberances of the other fold, and that the total surface of the vertices of the protrusions of said folds which participate in the connections represents at least 15% of the total surface of the vertices of the protuberances of said fold or the relative position of the patterns of the two folds. Feuille complexe selon la revendication 1, caractérisée par le fait qu'au moins 30 % des protubérances d'un pli participent à des liaisons effectives avec des protubérances coïncidentes de l'autre pli.Complex sheet according to claim 1, characterized in that at at least 30% of the protrusions of a fold participate in effective connections with coincident protuberances of the other fold. Feuille complexe selon la revendication 2, caractérisée par le fait qu'au moins 40 % des protubérances d'un pli participent à des liaisons effectives avec les protubérances coïncidentes et l'autre pli.Complex sheet according to claim 2, characterized in that at at least 40% of the protrusions of a fold participate in effective connections with the coincident protuberances and the other fold. Feuille complexe absorbante selon l'une quelconque des revendications 1 à 3, caractérisée par le fait que la surface totale liée des sommets des protubérances d'un pli est au moins égale à 20 % des surfaces des sommets des protubérances dudit pli.Absorbent complex sheet according to any one of Claims 1 to 3, characterized in that the total bonded area of the vertices of the protrusions of a fold is at least equal to 20% of the surfaces of the vertices of the protrusions of said fold. Feuille complexe selon l'une quelconque des revendications 1 à 4, caractérisée par le fait que la surface des sommets des protubérances de chaque pli est inférieure à 30 % de la surface totale dudit pli.Complex sheet according to any one of Claims 1 to 4, characterized by the fact that the surface of the vertices of the protrusions of each ply is less than 30% of the total area of said fold. Feuille complexe selon l'une des revendications 1 à 5, caractérisée par le fait que la surface des sommets des protubérances de chaque pli est supérieure à 7,5 % de la surface totale dudit pli.Complex sheet according to one of Claims 1 to 5, characterized in that that the surface of the vertices of the protrusions of each fold is greater than 7.5% of the total area of said fold. Feuille complexe selon la revendication 6, caractérisée par le fait que la surface des sommets des protubérances de chaque pli est inférieure à 15 % de la surface totale dudit pli. Complex sheet according to claim 6, characterized in that the surface of the peaks of the protrusions of each fold is less than 15% of the total area of said fold. Feuille complexe selon l'une quelconque des revendications 1 à 7, caractérisée par le fait que la densité des protubérances de chaque pli est inférieure à 20 protubérances par cm2.Complex sheet according to any one of Claims 1 to 7, characterized in that the density of the protuberances of each ply is less than 20 protuberances per cm 2 . Feuille complexe selon l'une quelconque des revendications 1 à 8, caractérisée par le fait que les deux plis sont gaufrés selon des motifs artistiques.Complex sheet according to any one of Claims 1 to 8, characterized by the fact that the two folds are embossed according to artistic patterns. Feuille complexe selon la revendication 9, caractérisée par le fait que les deux motifs artistiques sont identiques et décalés.Complex sheet according to claim 9, characterized in that the two artistic motifs are identical and offset. Feuille complexe selon la revendication 9, caractérisée par le fait que les deux motifs artistiques sont différents.Complex sheet according to claim 9, characterized in that the two artistic motifs are different.
    EP99400269A 1998-02-06 1999-02-05 Absorbent household paper Expired - Lifetime EP0935021B1 (en)

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    FR9801431A FR2774707B1 (en) 1998-02-06 1998-02-06 ABSORBENT PAPER FOR DOMESTIC USE
    FR9801431 1998-02-06

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    EA016514B1 (en) * 2007-07-13 2012-05-30 Джорджия - Пасифик Франс Creped absorbent paper sheet, roll for embossing such a sheet and embossing process
    US8216664B2 (en) 2007-07-13 2012-07-10 Georgia-Pacific France Creped absorbent paper sheet, roll for embossing such a sheet and embossing process

    Also Published As

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    TR199900240A2 (en) 1999-10-21
    ES2257014T3 (en) 2006-07-16
    ATE316168T1 (en) 2006-02-15
    NO990549D0 (en) 1999-02-05
    FR2774707B1 (en) 2000-04-07
    NO990549L (en) 1999-08-09
    DE69929506T2 (en) 2006-07-27
    DE69929506D1 (en) 2006-04-06
    DK0935021T3 (en) 2006-05-22
    FR2774707A1 (en) 1999-08-13
    TR199900240A3 (en) 1999-10-21
    PT935021E (en) 2006-05-31
    NO324478B1 (en) 2007-10-29
    EP0935021B1 (en) 2006-01-18
    CA2262020A1 (en) 1999-08-06
    US6235373B1 (en) 2001-05-22
    CA2262020C (en) 2007-05-01

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