EP1738025B1 - Structures fibreuses contenant une composition de traitement de surface et une composition de lotion - Google Patents

Structures fibreuses contenant une composition de traitement de surface et une composition de lotion Download PDF

Info

Publication number
EP1738025B1
EP1738025B1 EP05738715A EP05738715A EP1738025B1 EP 1738025 B1 EP1738025 B1 EP 1738025B1 EP 05738715 A EP05738715 A EP 05738715A EP 05738715 A EP05738715 A EP 05738715A EP 1738025 B1 EP1738025 B1 EP 1738025B1
Authority
EP
European Patent Office
Prior art keywords
fibrous structure
region
composition
structure according
lotion composition
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.)
Not-in-force
Application number
EP05738715A
Other languages
German (de)
English (en)
Other versions
EP1738025A1 (fr
Inventor
Joerg Kleinwaechter
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.)
Procter and Gamble Co
Original Assignee
Procter and Gamble Co
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Procter and Gamble Co filed Critical Procter and Gamble Co
Publication of EP1738025A1 publication Critical patent/EP1738025A1/fr
Application granted granted Critical
Publication of EP1738025B1 publication Critical patent/EP1738025B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
    • D21H25/02—Chemical or biochemical treatment
    • 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
    • D21H19/00—Coated paper; Coating material
    • D21H19/10—Coatings without pigments
    • 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

Definitions

  • the present invention relates to fibrous structures comprising a surface treating composition and a lotion composition, single- or multi-ply sanitary tissue products made therefrom and processes for making same. More particularly, the present invention relates to fibrous structures comprising a user contacting surface comprising a first region and a second region, wherein the first region comprises a first composition and the second region comprises a second composition different from the first composition. Even more particularly, the present invention relates to fibrous structures comprising a user contacting surface comprising a first region comprising a surface treating composition and a second region comprising a lotion composition.
  • Fibrous structures comprising a surface treating composition such as a softening composition and a lotion composition are known.
  • a surface treating composition such as a softening composition and a lotion composition
  • such conventional fibrous structures have utilized full coverage of a surface of the fibrous structure with the surface treating compositions and/or lotion compositions in an attempt to maximize transfer of the lotion composition.
  • Formulators have added an anti-migration material, such as a quaternary ammonium compound, into a fiber furnish such that the fibers are coated with the quaternary ammonium compound.
  • an anti-migration material such as a quaternary ammonium compound
  • the fibrous structure formed by the fiber furnish tends to mitigate the migration of a subsequently applied lotion composition into the fibrous structure.
  • the function of the quaternary ammonium compound and the level at which it is used are not provide softening of the fibrous structure surface.
  • WO 02/066740 discloses a lotioned and embossed tissue paper.
  • None of the known fibrous structures teach or suggest treating a surface of the fibrous structure with a surface treating composition and a lotion composition such that a user contacting surface comprising a first region comprising the surface treating composition and a second region comprising a lotion composition is produced on the surface of the fibrous structure.
  • a fibrous structure that comprises a surface treating composition such as a softening composition and a lotion composition such that a user contacting surface comprising a first region comprising the surface treating composition and a second region comprising the lotion composition is produced on a surface of the fibrous structure, a single- or multi-ply sanitary tissue product made therefrom and processes for making same.
  • a surface treating composition such as a softening composition
  • a lotion composition such that a user contacting surface comprising a first region comprising the surface treating composition and a second region comprising the lotion composition is produced on a surface of the fibrous structure, a single- or multi-ply sanitary tissue product made therefrom and processes for making same.
  • the present invention fulfills the needs described above by providing a fibrous structure and/or sanitary tissue product comprising a surface treating composition and a lotion composition such that a user contacting surface comprising a first region comprising the surface treating composition and a second region comprising the lotion composition is produced on a surface of the fibrous structure and/or sanitary tissue product.
  • a fibrous structure and/or single- or multi-ply sanitary tissue product comprising a user contacting surface wherein the user contacting surface comprises a first region comprising a surface treating composition and second region comprising a lotion composition is provided.
  • a fibrous structure and/or single- or multi-ply sanitary tissue product comprising a surface treating composition and a lotion composition, wherein the surface treating composition is present on a surface of the fibrous structure and/or single- or multi-ply sanitary tissue product at a greater level by weight than within the fibrous structure and/or single- or multi-ply sanitary tissue product and the lotion composition is present within the fibrous structure and/or single- or multi-ply sanitary tissue product at a greater level by weight than on the surface of the fibrous structure and/or single- or multi-ply sanitary tissue product, is provided.
  • Relative concentration of the surface treating composition and/or lotion composition on the surface can be determined using the Relative Concentration on Surface Test Method described herein.
  • a fibrous structure and/or single- or multi-ply sanitary tissue product comprising:
  • a single- or multi-ply sanitary tissue product comprising a fibrous structure according to the present invention is provided.
  • a process for treating a fibrous structure comprising the step of applying a lotion composition to a surface treating composition associated with a surface of a fibrous structure and/or single- or multi-ply sanitary tissue product, is provided.
  • a process for treating a fibrous structure and/or single- or multi-ply sanitary tissue product comprising the steps of:
  • a process for treating a fibrous structure and/or single- or multi-ply sanitary tissue product comprising the steps of:
  • the present invention provides fibrous structures and/or single- or multi-ply sanitary tissue products comprising a surface treating composition and a lotion composition, products made therefrom and processes for making same.
  • Fiber as used herein means an elongate particulate having an apparent length greatly exceeding its apparent diameter, i.e. a length to diameter ratio of at least about 10. Fibers having a non-circular cross-section are common; the "diameter” in this case may be considered to be the diameter of a circle having cross-sectional area equal to the cross-sectional area of the fiber. More specifically, as used herein, “fiber” refers to papermaking fibers. The present invention contemplates the use of a variety of papermaking fibers, such as, for example, natural fibers or synthetic fibers, or any other suitable fibers, and any combination thereof.
  • Natural papermaking fibers useful in the present invention include animal fibers, mineral fibers, plant fibers and mixtures thereof.
  • Animal fibers may, for example, be selected from the group consisting of: wool, silk and mixtures thereof.
  • Plant fibers may, for example, be derived from a plant selected from the group consisting of: wood, cotton, cotton linters, flax, sisal, abaca, hemp, hesperaloe, jute, bamboo, bagasse, kudzu, corn, sorghum, gourd, agave, loofah and mixtures thereof.
  • Wood fibers include chemical pulps, such as kraft (sulfate) and sulfite pulps, as well as mechanical and semi-chemical pulps including, for example, groundwood, thermomechanical pulp, chemi-mechanical pulp (CMP), chemithermomechanical pulp (CTMP), neutral semi-chemical sulfite pulp (NSCS). Chemical pulps, however, may be preferred since they impart a superior tactile sense of softness to tissue sheets made therefrom. Pulps derived from both deciduous trees (hereinafter, also referred to as "hardwood”) and coniferous trees (hereinafter, also referred to as "softwood”) may be utilized.
  • hardwood deciduous trees
  • softwood coniferous trees
  • the hardwood and softwood fibers can be blended, or alternatively, can be deposited in layers to provide a stratified and/or layered fibrous structure.
  • U.S. Pat. Nos. 4,300,981 and U.S. Pat. No. 3,994,771 disclose layering of hardwood and softwood fibers.
  • fibers derived from recycled paper which may contain any or all of the above categories as well as other non-fibrous materials such as fillers and adhesives used to facilitate the original papermaking.
  • the wood pulp fibers may be short (typical of hardwood fibers) or long (typical of softwood fibers).
  • short fibers include fibers derived from a fiber source selected from the group consisting of Acacia, Eucalyptus, Maple, Oak, Aspen, Birch, Cottonwood, Alder, Ash, Cherry, Elfin, Hickory, Poplar, Gum, Walnut, Locust, Sycamore, Beech, Catalpa, Sassafras, Gmelina, Albizia, Anthocephalus, and Magnolia.
  • long fibers include fibers derived from Pine, Spruce, Fir, Tamarack, Hemlock, Cypress, and Cedar.
  • Softwood fibers derived from the kraft process and originating from more-northern climates may be preferred. These are often referred to as northern softwood kraft (NSK) pulps.
  • Synthetic fibers may be selected from the group consisting of: wet spun fibers, dry spun fibers, melt spun (including melt blown) fibers, synthetic pulp fibers and mixtures thereof.
  • Synthetic fibers may, for example, be comprised of cellulose (often referred to as "rayon”); cellulose derivatives such as esters, ether, or nitrous derivatives; polyolefins (including polyethylene and polypropylene); polyesters (including polyethylene terephthalate); polyamides (often referred to as "nylon”); acrylics; non-cellulosic polymeric carbohydrates (such as starch, chitin and chitin derivatives such as chitosan); and mixtures thereof.
  • Fibrous structure as used herein means a structure that comprises one or more fibers.
  • processes for making fibrous structures include known wet-laid papermaking processes and air-laid papermaking processes. Such processes typically include steps of preparing a fiber composition, oftentimes referred to as a fiber slurry in wet-laid processes, either wet or dry, and then depositing a plurality of fibers onto a forming wire or belt such that an embryonic fibrous structure is formed, drying and/or bonding the fibers together such that a fibrous structure is formed, and/or further processing the fibrous structure such that a finished fibrous structure is formed.
  • the finished fibrous structure is the fibrous structure that is wound on the reel at the end of papermaking, but before converting thereof into a sanitary tissue product.
  • “Sanitary tissue product” comprises one or more fibrous structures, converted or not, that is useful as a wiping implement for post-urinary and post-bowel movement cleaning (toilet tissue), for otorhinolaryngological discharges (facial tissue and/or disposable handkerchiefs), and multi-functional absorbent and cleaning uses (absorbent towels and/or wipes).
  • toilet tissue post-urinary and post-bowel movement cleaning
  • facial tissue and/or disposable handkerchiefs for otorhinolaryngological discharges
  • multi-functional absorbent and cleaning uses as absorbent towels and/or wipes.
  • a lotion composition-containing multi-ply disposable handkerchief having a caliper of from about 0.1 mm to about 0.4 mm in accordance with the present invention is provided.
  • Ply or Plies as used herein means an individual finished fibrous structure optionally to be disposed in a substantially contiguous, face-to-face relationship with other plies, forming a multiple ply finished fibrous structure product and/or sanitary tissue product. It is also contemplated that a single fibrous structure can effectively form two "plies” or multiple "plies", for example, by being folded on itself.
  • “Surface of a fibrous structure” as used herein means that portion of the fibrous structure that is exposed to the external environment.
  • the surface of a fibrous structure is that portion of the fibrous structure that is not completely surrounded by other portions of the fibrous structure.
  • “User Contacting Surface” as used herein means that portion of the fibrous structure and/or surface treating composition and/or lotion composition present directly and/or indirectly on the surface of the fibrous structure that is exposed to the external environment. In other words, it is that surface formed by the fibrous structure including any surface treating composition and/or lotion composition present directly and/or indirectly on the surface of the fibrous structure that contacts an opposing surface when used by a user. For example, it is that surface formed by the fibrous structure including any surface treating composition and/or lotion composition present directly and/or indirectly on the surface of the fibrous structure that contacts a user's skin when a user wipes his/her skin with the fibrous structure of the present invention.
  • the user contacting surface especially for a textured and/or structured fibrous structure, such as a through-air-dried fibrous structure and/or an embossed fibrous structure, may comprise raised areas and recessed areas of the fibrous structure.
  • the raised areas may be knuckles and the recessed areas may be pillows and vice versa.
  • the knuckles may, directly and/or indirectly, comprise the lotion composition and the pillows may comprise the surface treating composition and vice versa so that when a user contacts the user's skin with the fibrous structure, the lotion composition and surface treating composition both contact the user's skin.
  • embossed fibrous structures with the embossed areas may, directly and/or indirectly, comprise the lotion composition and the non-embossed areas may comprise the surface treating composition and vice versa.
  • the user contacting surface has to comprise regions of sufficient size such that two or more different regions (comprising different compositions) are exposed to an opposing surface during use.
  • a surface of a fibrous structure that is substantially covered (on a microscopic scale) by a lotion composition but completely covered on a macro scale by such lotion composition such that a user's skin is only contacted by the lotion composition does not contain two different regions in its user contacting surface.
  • a user contacting surface may comprise an external layer of a multi-layer fibrous structure wherein the external layer may comprise a surface treating composition and/or a lotion composition.
  • the user contacting surface may be present on the fibrous structure and/or sanitary tissue product before use by the user and/or the user contacting surface may be created/formed prior to and/or during use of the fibrous structure and/or sanitary tissue product by the user, such as upon the user applying pressure to the fibrous structure and/or sanitary tissue product as the user contacts the user's skin with the fibrous structure and/or sanitary tissue product.
  • component or composition levels are in reference to the active level of that component or composition, and are exclusive of impurities, for example, residual solvents or by-products, which may be present in commercially available sources.
  • Fig. 1 is a schematic representation of a fibrous structure in accordance with the present invention.
  • a fibrous structure 10 comprising a user contacting surface 12 comprising a first region 14 and a second region 16.
  • the user contacting surface 12 is associated with a surface of the fibrous structure 18.
  • the surface of the fibrous structure 18 may comprise one or more fibers 20.
  • the first region 14 and/or second region 16 may be present on (associated with) the surface of the fibrous structure 18.
  • first region 14 and/or the second region 16 are present on the surface of the fibrous structure 18, one or both may be present on the surface of the fibrous structure 18 in the form of a continuous or substantially continuous network and/or in a plurality of discrete areas (also sometimes known as "islands").
  • the first region 14 and/or the second region 16 may be in contact with and/or cover the entire or substantially the entire surface area of the surface of the fibrous structure 18.
  • the first region 14 is in contact with and/or covers the entire or substantially the entire surface area of the surface of the fibrous structure 18.
  • the first region 14 and/or the second region 16 may be in contact with and/or cover less than the entire or substantially the entire surface area of the surface of the fibrous structure 18.
  • the second region 16 is in contact with and/or covers less than the entire or substantially the entire surface area of the surface of the fibrous structure 18.
  • that region may be in the form of a plurality of discrete areas.
  • the first region 14 is in contact with and/or covers substantially the entire surface area of the surface of the fibrous structure 18 and the second region 16 is in contact with and/or covers less than substantially the entire surface area of the surface of the fibrous structure 18.
  • the first region 14 may be in the form of a continuous or substantially continuous network and the second region 16 may be in the form of a plurality of discrete areas dispersed throughout the continuous or substantially continuous network of the first region 14.
  • Either region may be in contact with the other region.
  • the second region 16 is in contact with the first region 14 such that the first region 14 is positioned between the second region 16 and the surface of the fibrous structure 18.
  • the second region 16 may be present on less than the entire surface area of the first region 14.
  • the second region 16 may be present on the first region 14 in the form of one or more discrete areas.
  • portions of the second region 16 are in contact with the first region 14 such that both the second region 16 and the first region 14 are in contact directly with the surface of the fibrous structure 18. Also as shown in Figs. 4 and 5 , a portion of the second region 16 is not in contact with the first region 14.
  • Figs. 4 and 5 also show that less than substantially the entire surface area of the surface of the fibrous structure 18 is in contacted by or covered by the first region 14 and the second region 16.
  • the user contacting surface 12 comprises a third region, namely, the surface of the fibrous structure 18 as well as the first region 14 and the second region 16.
  • Fig. 6 is a schematic representation of another example of a fibrous structure in accordance with the present invention.
  • the fibrous structure 10 comprises a user contacting surface 12 that comprises a first region 14, a second region 16 and a third region, in this case, the surface of the fibrous structure 18 which comprises one or more fibers 20.
  • the first region 14 comprises a surface treating composition.
  • the second region 16 comprises a lotion composition.
  • the surface treating composition and/or lotion composition may be present on the surface of the fibrous structure 18 at a greater level by weight than within the fibrous structure.
  • the surface treating composition and/or lotion composition may be present within the fibrous structure at a greater level by weight than on the surface of the fibrous structure 18.
  • the surface area coverage of the surface treating composition on the surface of the fibrous structure may be greater than about 10% and/or greater than about 30% and/or greater than about 50% to about 100% and/or to about 90% and/or to about 85%.
  • the surface area coverage of the lotion composition on the surface of the fibrous structure may be may be greater than about 1% and/or greater than about 5% and/or greater than about 10% and/or greater than about 20% to about 99% and/or to about 90% and/or to about 75% and/or to about 50%.
  • the surface area of the fibrous structure and/or sanitary tissue product comprises greater than about 10% and/or greater than about 20% and/or greater than about 50% and/or greater than about 70% and/or greater than about 80% and/or greater than about 90% of the surface treating composition and from 0 to about 90% and/or from 0 to about 80% and/or from 0 to about 50% and/or from 0 to about 30% and/or from 0 to about 20% and/or from 0 to about 10% of the lotion composition.
  • the surface area of the surface of the fibrous structure and/or sanitary tissue product comprises 0% of the lotion composition
  • the lotion may be within the fibrous structure and/or within the sanitary tissue product, such as between two plies of the sanitary tissue product.
  • the surface area of the user contacting surface comprises from about 20% to about 97% and/or from about 50% to about 97% and/or from about 80% to about 97% of the surface treating composition and from about 3% to about 80% and/or from about 3% to about 50% and/or from about 3% to about 20% and/or from about 3% to about 15% of the lotion composition.
  • Surface area coverage of the fibrous structure and/or sanitary tissue product may be determined by the Surface Area Coverage Test Method described herein.
  • Each region may, within itself, exhibit differential concentrations of their respective compositions and/or differential elevations (protrusions from the surface of the fibrous structure) of their respective compositions
  • the user contacting surface area may comprise from greater than about 10% and/or greater than about 30% and/or greater than about 50% to about 100% and/or to about 90% and/or to about 85% of the surface treating composition and/or greater than about 1% and/or greater than about 5% and/or greater than about 10% and/or greater than about 20% to about 99% and/or to about 90% and/or to about 75% and/or to about 50% of the lotion composition.
  • the combination of the surface treating composition and lotion composition in the user contacting surface exhibits softness greater than a user contacting surface comprising either the surface treating composition or lotion composition alone.
  • the user contacting surface may be planar or may have protrusions of either the surface treating composition and/or lotion composition such that the user contacting surface exhibits differential elevations.
  • the user contacting surface may comprise areas of greater concentration and/or greater elevation of the lotion composition, areas of less concentration and/or lesser elevation of the lotion composition, and areas of the surface treating composition.
  • the surface treating composition and the lotion composition may comprise one or more similar and/or identical ingredients so long as the user contacting surface comprises a first region comprising a different composition (at least one ingredient differs in the composition) than a composition present in a second region.
  • Nonlimiting types of fibrous structures according to the present invention include conventionally felt-pressed fibrous structures; pattern densified fibrous structures; and high-bulk, uncompacted fibrous structures.
  • the fibrous structures may be of a homogeneous or multilayered (two or three or more layers) construction; and the sanitary tissue products made therefrom may be of a single-ply or multi-ply construction.
  • the fibrous structures may be post-processed, such as by embossing and/or calendaring and/or folding and/or printing images thereon.
  • the fibrous structures may be through-air-dried fibrous structures or conventionally dried fibrous structures.
  • the fibrous structures may be creped or uncreped.
  • the fibrous structures and/or sanitary tissue products of the present invention may exhibit a basis weight of between about 10 g/m 2 to about 120 g/m 2 and/or from about 12 g/m 2 to about 80 g/m 2 and/or from about 14 g/m 2 to about 65 g/m 2 .
  • the fibrous structures and/or sanitary tissue products of the present invention may exhibit a total dry tensile strength of greater than about 59 g/cm (150 g/in) and/or from about 78 g/cm (200 g/in) and/or from about 98 g/cm (250 g/in) to about 1182 g/cm (3000 g/in) and/or to about 984 g/cm (2500 g/in) and/or to about 787 g/cm (2000 g/in) and/or to about 394 g/cm (1000 g/in) and/or to about 335 g/cm (850 g/in).
  • the fibrous structure and/or sanitary tissue products of the present invention may exhibit a density of less than about 0.60 g/cm 3 and/or less than about 0.30 g/cm 3 and/or less than about 0.20 g/cm 3 and/or less than about 0.10 g/cm 3 and/or less than about 0.07 g/cm 3 and/or less than about 0.05 g/cm 3 and/or from about 0.01 g/cm 3 to about 0.20 g/cm 3 and/or from about 0.02 g/cm 3 to about 0.10 g/cm 3 .
  • the fibrous structures and/or sanitary tissue products of the present invention may exhibit an average lint value of greater than about 0.1 and/or greater than about 0.5 and/or greater than about 1.0 and/or greater than about 1.5 and/or greater than about 2.0 and/or greater than about 3.0 to about 20 and/or to about 15 and/or to about 13 and/or to about 10 and/or to about 8.
  • a surface treating composition for purposes of the present invention, is a composition that improves the tactile sensation of a surface of a fibrous structure perceived by a user whom holds a fibrous structure and/or sanitary tissue product comprising the fibrous structure and rubs it across the user's skin.
  • Such tactile perceivable softness can be characterized by, but is not limited to, friction, flexibility, and smoothness, as well as subjective descriptors, such as a feeling like lubricious, velvet, silk or flannel.
  • the surface treating composition may or may not be transferable. Typically, it is substantially non-transferable.
  • the surface treating composition may increase or decrease the surface friction of the surface of the fibrous structure, especially the user contacting surface of the fibrous structure.
  • the surface treating composition will reduce the surface friction of the surface of the fibrous structure compared to a surface of the fibrous structure without such surface treating composition.
  • the surface treating composition may have a wettability tension less than or equal to the surface tension of the lotion composition so as to minimize the spreading of the lotion composition that comes into contact with the surface treating composition.
  • the surface treating composition comprises a surface treating agent.
  • the surface treating composition during application to the fibrous structure may comprise at least about 0.1% and/or at least 0.5% and/or at least about 1% and/or at least about 3% and/or at least about 5% to about 90% and/or to about 80% and/or to about 70% and/or to about 50% and/or to about 40% by weight of the surface treating agent.
  • the surface treating composition comprises from about 5% to about 40% by weight of the surface treating agent.
  • the surface treating composition present on the fibrous structure and/or sanitary tissue product comprising the fibrous structure of the present invention may comprise at least about 0.01% and/or at least about 0.05% and/or at least about 0.1% of total basis weight of the surface treating agent.
  • the fibrous structure and/or sanitary tissue product may comprise from about 0.01% to about 20% and/or from about 0.05% to about 15% and/or from about 0.1% to about 10% and/or from about 0.01% to about 5% and/or from about 0.1% to about 2% of total basis weight of the surface treating composition.
  • the surface treating composition of the present invention is a microemulsion of a surface treating agent (for example an aminofunctional polydimethylsiloxane) in water.
  • a surface treating agent for example an aminofunctional polydimethylsiloxane
  • the concentration of the surface treating agent within the surface treating composition may be from about 3% to about 60% and/or from about 4% to about 50% and/or from about 5% to about 40%.
  • Nonlimiting examples of such microemulsions are commercially available from Wacker Chemie, Dow Corning and/or General Electric Silicones.
  • Nonlimiting examples of suitable surface treating agents are selected from the group consisting of: polymers such as polyethylene and derivatives thereof, hydrocarbons, waxes, oils, silicones (polysiloxanes), quaternary ammonium compounds, fluorocarbons, substituted C 10 -C 22 alkanes, substituted C 10 -C 22 alkenes, in particular derivatives of fatty alcohols and fatty acids(such as fatty acid amides, fatty acid condensates and fatty alcohol condensates), polyols, derivatives of polyols (such as esters and ethers), sugar derivatives (such as ethers and esters), polyglycols (such as polyethyleneglycol) and mixtures thereof.
  • polymers such as polyethylene and derivatives thereof, hydrocarbons, waxes, oils, silicones (polysiloxanes), quaternary ammonium compounds, fluorocarbons, substituted C 10 -C 22 alkanes, substituted C 10 -C 22 al
  • Nonlimiting examples of suitable waxes may be selected from the group consisting of: paraffin, polyethylene waxes, beeswax and mixtures thereof.
  • Nonlimiting examples of suitable oils may be selected from the group consisting of: mineral oil, silicone oil, silicone gels, petrolatum and mixtures thereof.
  • Nonlimiting examples of suitable silicones may be selected from the group consisting of: polydimethylsiloxanes, aminosilicones, cationic silicones, quaternary silicones, silicone betaines and mixtures thereof.
  • Nonlimiting examples of suitable polysiloxanes and/or monomeric/oligomeric units may be selected from the compounds having monomeric siloxane units of the following structure: wherein, R 1 and R2, for each independent siloxane monomeric unit can each independently be hydrogen or any alkyl, aryl, alkenyl, alkaryl, arakyl, cycloalkyl, halogenated hydrocarbon, or other radical. Any of such radical can be substituted or unsubstituted. R 1 and R 2 radicals of any particular monomeric unit may differ from the corresponding functionalities of the next adjoining monomeric unit. Additionally, the polysiloxane can be either a straight chain, a branched chain or have a cyclic structure.
  • the radicals R 1 and R 2 can additionally independently be other silaceous functionalities such as, but not limited to siloxanes, polysiloxanes, silanes, and polysilanes.
  • the radicals R 1 and R 2 may contain any of a variety of organic functionalities including, for example, alcohol, carboxylic acid, phenyl, and amine functionalities.
  • the end groups can be reactive (alkoxy or hydroxyl) or nonreactive (trimethylsiloxy).
  • the polymer can be branched or unbranched.
  • Exemplary alkyl radicals are methyl, ethyl, propyl, butyl, pentyl, hexyl, octyl, decyl, octadecyl, and the like.
  • Exemplary alkenyl radicals are vinyl, allyl, and the like.
  • Exemplary aryl radicals are phenyl, diphenyl, naphthyl, and the like.
  • Exemplary alkaryl radicals are toyl, xylyl, ethylphenyl, and the like.
  • Exemplary aralkyl radicals are benzyl, alpha-phenylethyl, beta-phenylethyl, alpha-phenylbutyl, and the like.
  • Exemplary cycloalkyl radicals are cyclobutyl, cyclopentyl, cyclohexyl, and the like.
  • Exemplary halogenated hydrocarbon radicals are chloromethyl, bromoethyl, tetrafluorethyl, fluorethyl, trifluorethyl, trifluorotloyl, hexafluoroxylyl, and the like.
  • Viscosity of polysiloxanes useful for this invention may vary as widely as the viscosity of polysiloxanes in general vary, so long as the polysiloxane can be rendered into a form which can be applied to the fibrous structures herein. This includes, but is not limited to, viscosity as low as about 25 centistokes to about 20,000,000 centistokes or even higher.
  • Nonlimiting examples of suitable quaternary ammonium compounds may be selected from compounds having the formula: wherein:
  • each R 1 is methyl and X - is chloride or methyl sulfate and each R 2 is independently C 16 -C 18 alkyl or alkenyl. Each R 2 may be independently straight-chain C 18 alkyl or alkenyl.
  • the quaternary ammonium compounds may be mono or diester variations having the formula: (R 1 ) 4-m -N+-[(CH 2 ) n -Y-R 3 ] m X - wherein:
  • the quaternary ammonium compound may be an imidazolinium compound, such as an imidazolinium salt.
  • X - can be any quaternary ammonium-compatible anion, for example, acetate, chloride, bromide, methyl sulfate, formate, sulfate, nitrate and the like can also be used in the present invention.
  • X - is chloride or methyl sulfate.
  • the surface treating composition may comprise additional ingredients such as a vehicle as described herein below which may not be present on the fibrous structure and/or sanitary tissue product comprising such fibrous structure.
  • the surface treating composition may comprise a surface treating agent and a vehicle such as water to facilitate the application of the surface treating agent onto the surface of the fibrous structure.
  • the lotion composition may comprise oils and/or emollients and/or waxes and/or immobilizing agents.
  • the lotion composition comprises from about 10% to about 90% of an oil and/or liquid emollient and from about 10% to about 50% of immobilizing agent and/or from about 0% to about 60% of petrolatum and optionally the balance of a vehicle.
  • the lotion compositions may be heterogeneous. They may contain solids, gel structures, polymeric material, a multiplicity of phases (such as oily and water phase) and/or emulsified components. It may be difficult to determine precisely the melting temperature of the lotion composition, i.e. difficult to determine the temperature of transition between the liquid form, the quasi-liquid from, the quasi-solid form and the solid form.
  • melting temperature, melting point, transition point and transition temperature are used interchangeably in this document and have the same meaning.
  • the lotion compositions may be semi-solid, of high viscosity so they do not substantially flow without activation during the life of the product or gel structures.
  • the lotion compositions may be shear thinning and/or they may strongly change their viscosity around skin temperature to allow for transfer and easy spreading on a user's skin.
  • the lotion compositions may be in the form of emulsions and/or dispersions.
  • the lotion composition has a water content of less than about 20% and/or less than 10% and/or less than about 5% or less than about 0.5%.
  • the lotion composition may have a solids content of at least about 15% and/or at least about 25% and/or at least about 30% and/or at least about 40% to about 100% and/or to about 95% and/or to about 90% and/or to about 80%.
  • Nonlimiting examples of suitable oils and/or emollients include glycols (such as propylene glycol and/or glycerine), polyglycols (such as triethylene glycol), petrolatum, fatty acids, fatty alcohols, fatty alcohol ethoxylates, fatty alcohol esters and fatty alcohol ethers, fatty acid ethoxylates, fatty acid amides and fatty acid esters, hydrocarbon oils (such as mineral oil), squalane, fluorinated emollients, silicone oil (such as dimethicone) and mixtures thereof.
  • glycols such as propylene glycol and/or glycerine
  • polyglycols such as triethylene glycol
  • petrolatum such as propylene glycol and/or glycerine
  • fatty acids such as propylene glycol and/or glycerine
  • fatty alcohol ethoxylates such as fatty alcohol esters and fatty alcohol ethers
  • Suitable fatty acid ester type emollients include those derived from C 12 -C 28 fatty acids, such as C 16 -C 22 saturated fatty acids, and short chain (C 1 -C 8 and/or C 1 -C 3 ) monohydric alcohols.
  • Representative examples of such esters include methyl palmitate, methyl stearate, isopropyl laurate, isopropyl myristate, isopropyl palmitate, and ethylhexyl palmitate.
  • Suitable fatty acid ester emollients can also be derived from esters of longer chain fatty alcohols (C 12 -C 28 and/or C 12 -C 16 ) and shorter chain fatty acids e.g., lactic acid, such as lauryl lactate and cetyl lactate.
  • Suitable alkyl ethoxylate type emollients include C 12 -C 18 fatty alcohol ethoxylates having an average of from about 3 to about 30 and/or from about 4 to about 23 oxyethylene units.
  • alkyl ethoxylates include laureth-3 (a lauryl ethoxylate having an average of 3 oxyethylene units), laureth-23 (a lauryl ethoxylate having an average of 23 oxyethylene units), ceteth-10 (acetyl ethoxylate having an average of 10 oxyethylene units) and steareth-10 (a stearyl ethoxylate having an average of 10 oxyethylene units).
  • alkyl ethoxylate emollients can be used in combination with other emollients, such as petroleum-based emollients, such as petrolatum, at a weight ratio of alkyl ethoxylate emollient to petroleum-based emollient of from about 1:1 to about 1:3 and/or from about 1:1.5 to about 1:2.5.
  • petroleum-based emollients such as petrolatum
  • Immobilizing agents include agents that are may prevent migration of the emollient into the fibrous structure such that the emollient remain primarily on the surface of the fibrous structure and/or sanitary tissue product and/or on the surface treating composition on a surface of the fibrous structure and/or sanitary tissue product and facilitate transfer of the lotion composition to a user's skin. Immobilizing agents may function as viscosity increasing agents and/or gelling agents.
  • suitable immobilizing agents include waxes (such as ceresin wax, ozokerite, microcrystalline wax, petroleum waxes, fisher tropsh waxes, silicone waxes, paraffin waxes), fatty alcohols (such as cetyl and/or stearyl alcohol), fatty acids and their salts (such as metal salts of stearic acid), mono and polyhydroxy fatty acid esters, mono and polyhydroxy fatty acid amides, silica and silica derivatives, gelling agents, thickeners and mixtures thereof.
  • waxes such as ceresin wax, ozokerite, microcrystalline wax, petroleum waxes, fisher tropsh waxes, silicone waxes, paraffin waxes
  • fatty alcohols such as cetyl and/or stearyl alcohol
  • fatty acids and their salts such as metal salts of stearic acid
  • mono and polyhydroxy fatty acid esters such as ceresin wax, ozokerite, microcrystalline wax, petroleum waxes, fisher tropsh
  • the lotion composition comprises at least one immobilizing agent and at least one emollient.
  • the lotion composition comprises a sucrose ester of a fatty acid.
  • the lotion composition may be added to a fibrous structure at any point during the papermaking and/or converting process. In one example, the lotion composition is added to the fibrous structure during the converting process.
  • the lotion composition may be a transferable lotion composition.
  • a transferable lotion composition comprises at least one component that is capable of being transferred to an opposing surface such as a user's skin upon use. In one example, at least 0.1% of the transferable lotion present on the user contacting surface transfers to the user's skin during use.
  • the amount of transferable composition that transfers to a user's skin during use can be determined by known methods such as by tape stripping the skin 3 times, after use of the fibrous structure and/or sanitary tissue product by the user, with Tegaderm Tapes, available from 3M, and analyzing the tapes for the transferable composition or a component within the transferable composition assuming all components of the transferable composition transfer equally.
  • lotion composition components include vehicles, perfumes, especially long lasting and/or enduring perfumes, antibacterial actives, antiviral actives, disinfectants, pharmaceutical actives, film formers, deodorants, opacifiers, astringents, solvents, cooling sensate agents, and the like.
  • lotion composition components include camphor, thymol, menthol, chamomile extracts, aloe vera, calendula officinalis, alpha bisalbolol, Vitamin E, Vitamin E acetate.
  • the lotion composition has a melting point greater than about 35°C.
  • the lotion composition has to be subjected to a temperature of greater than about 35°C before a substantial amount (for example, greater than 30% and/or greater than 40% and/or greater than 50% and/or greater than 60%) of the lotion composition melts. This can be expressed as:
  • ⁇ H is measured by DSC technique using standard parameters known to the one skilled in the art.
  • DSC data are obtained using a Thwing Albert DSC 2920 Instrument, calibrated with an indium metal standard with a melting onset temperature of 156.6°C and a heat of melting of 6.80 calories per gram, as reported in the literature. The sample is first heated to 100°C at a rate of 10°C/min, equilibrated for 5 minutes at 100°C, cooled down to -30°C at a rate of -2.5°C/min, equilibrated at -30°C for 5 minutes and then finally heated from -30°C to +100°C at a rate of 2.5°C/min to evaluate the melt behaviour.
  • ⁇ H 1 and ⁇ H 2 are the areas between the DSC curve and the baseline between 15°C and 35°C and ⁇ H 2 is the area between the DSC curve and the baseline between 35°C and the temperature where the lotion composition is fully liquid or where no more melting occurs below 100°C in the case the lotion composition contains components only melting above 100°C.
  • a lotion composition of the present invention that comprises about 40% Stearylalcohol, about 30% Mineral oil and about 30% Petrolatum has a value of ⁇ H 2 / ⁇ H 1 > 9 and a value of ⁇ H 2 > 60J/g.
  • the lotion composition is present on the surface of the fibrous structure and/or sanitary tissue product and/or on the surface treating composition present on the surface of the fibrous structure and/or sanitary tissue product at a level of at least about 0.5 g/m 2 and/or at least about 1.0 g/m 2 and/or at least about 1.5 g/m 2 per user contacting surface.
  • the lotion composition is present on the surface of the fibrous structure and/or sanitary tissue product and/or on the surface treating composition present on the surface of the fibrous structure and/or sanitary tissue product at a level of from about 0.5 g/m 2 and/or from about 1.0 g/m 2 and/or from about 1.5 g/m 2 to about 10 g/m 2 and/or to about 8 g/m 2 and/or to about 6 g/m 2 per user contacting surface.
  • a "vehicle” is a material that can be used to dilute and/or emulsify agents forming the surface treating composition and/or lotion composition to form a dispersion/emulsion.
  • a vehicle may be present in the surface treating composition and/or lotion composition, especially during application of the surface treating composition and/or to the fibrous structure.
  • a vehicle may dissolve a component (true solution or micellar solution) or a component may be dispersed throughout the vehicle (dispersion or emulsion).
  • the vehicle of a suspension or emulsion is typically the continuous phase thereof. That is, other components of the dispersion or emulsion are dispersed on a molecular level or as discrete particles throughout the vehicle.
  • Suitable materials for use as the vehicle of the present invention include hydroxyl functional liquids, including but not limited to water.
  • the lotion composition comprises less than about 20% and/or less than about 10% and/or less than about 5% and/or less than about 0.5% w/w of a vehicle, such as water.
  • the surface treating composition comprises greater than about 50% and/or greater than about 70% and/or greater than about 85% and/or greater than about 95% and/or greater than about 98% w/w of a vehicle, such as water.
  • Process aids may also be used in the lotion compositions of the present invention.
  • suitable process aids include brighteners, such as TINOPAL CBS-X ® , obtainable from CIBA-GEIGY of Greensboro, N.C.
  • the lotion composition has a melting point of about 51°C and a melt viscosity at 56°C of about 17 m*Pas measured at a shear rate of 0.1 1/s.
  • the mineral oil used in this formulation has a viscosity of about 21 mPa*s at 20°C.
  • the lotion composition can be applied to one or both surfaces of the fibrous structure at total add-on levels of 3.6g/m 2 , 4.2g/m 2 , 6g/m 2 , 7.2g/m 2 , 8.4g/m 2 and 11.4g/m 2 .
  • any contact or contact free application suitable for applying the surface treating composition such as spraying, dipping, padding, printing, slot extruding, rotogravure printing, flexographic printing, offset printing, screen printing, mask or stencil application process and mixtures thereof can be used to apply the surface treating composition to the fibrous structure and/or sanitary tissue product and/or to the lotion composition present on a surface of the fibrous structure and/or sanitary tissue product.
  • Surface treating compositions can be applied to the fibrous structure and/or sanitary tissue product before, concurrently, or after the lotion composition application to the fibrous structure and/or sanitary tissue product.
  • the surface treating composition can be applied during papermaking and/or converting, especially if applied to the outside layer of a layered fibrous structure and/or sanitary tissue product comprising such layered fibrous structure.
  • the surface treating composition is applied by an application process that provides a relatively high surface area coverage on the surface of the fibrous structure and/or sanitary tissue product.
  • suitable application process include, but are not limited to, printing, slot extruding and/or spraying with fine particles (although spraying has disadvantage of producing aerosoles if high area coverage is to be achieved).
  • any contact or contact free application suitable for applying the lotion composition such as spraying, dipping, padding, printing, slot extruding, rotogravure printing, flexographic printing, offset printing, screen printing, mask or stencil application process and mixtures thereof can be used to apply the lotion composition to the fibrous structure and/or sanitary tissue product and/or surface treating composition present on the surface of the fibrous structure and/or sanitary tissue product.
  • the lotion composition can be applied to the fibrous structure and/or sanitary tissue product before, concurrently, and/or after the surface treating composition application to the fibrous structure and/or sanitary tissue product.
  • the lotion composition is applied to the surface treating composition present on the surface of the fibrous structure and/or sanitary tissue product.
  • the lotion composition is applied by an application process that provides a relatively low surface area coverage on the surface of the fibrous structure and/or sanitary tissue product and/or on the surface treating composition present on the surface of the fibrous structure and/or sanitary tissue product such that regions of surface treating composition and regions of lotion composition produce the user contacting surface.
  • suitable application processes include, but are not limited to, spraying, especially spraying with rotating discs, printing, slot extruding in stripes and/or other patterns.
  • the surface treating composition may be added to a fiber furnish that will form an external layer of a multilayer fibrous structure.
  • the lotion composition may be applied to the surface formed by the external layer of the multilayer fibrous structure.
  • the surface treating composition is applied to the surface of the fibrous structure during the fibrous structure making process, such as before and/or after drying the fibrous structure.
  • the lotion composition may then be applied to the surface treating composition on the surface of the fibrous structure during the converting process.
  • the surface treating composition contains less than about 5% and/or less than about 3% and/or less than about 1% and/or less than about 0.5% moisture at the time the lotion composition is applied to it.
  • a first fibrous structure is a conventional wet pressed, homogeneous, dry creped fibrous structure with a basis weight of about 15.4 g/m 2 .
  • the fibrous structure has a composition of about 40% Northern Softwood Kraft and 60% Eucalyptus.
  • Four plies of the fibrous structure are combined together in an off line combining operation to produce a sanitary tissue product.
  • the 4-ply sanitary tissue product has a basis weight of about 60g/m 2 , a thickness of about 0.3 mm, a machine direction strength of about 1280 g/2.54cm (1280 g/in), a cross direction strength of about 610 g/2.54cm (610 g/in), and a wet burst of about 200g. It contains a wet strength agent and a dry strength agent.
  • a second fibrous structure is a conventional wet pressed, layered, dry creped fibrous structure with a basis weight of about 14.6 g/m 2 .
  • the outer layer contains about 100% Eucalyptus fiber whereas the inner layer is composed of a furnish mix of about 85% Northern Softwood Kraft, 10% CTMP and about 5% Eucalyptus fiber. Both layers are of about equal basis weight (symmetrical layer split).
  • Four plies of the fibrous structure are combined together in an off line combining operation to form a sanitary tissue product such that the Eucalyptus layer is present on the two outer surfaces of the combined 4-ply sanitary tissue product.
  • the 4-ply sanitary tissue product has a basis weight of about 60g/m 2 , a thickness of about 0.3 mm, a machine direction strength of about 1180 g/2.54cm (1180 g/in), a cross direction strength of about 560 g/2.54cm (560 g/in), and a wet burst of about 200g. It contains a wet strength agent and a dry strength agent.
  • a third fibrous structure is formed from an aqueous slurry of Northern Softwood Kraft (NSK) of about 3% consistency made up using a conventional pulper and passed through a stock pipe toward the headbox of the Fourdrinier.
  • NSK Northern Softwood Kraft
  • a 1% dispersion of Hercules' Kymene 557 LX is prepared and is added to the NSK stock pipe at a rate sufficient to deliver about 0.8% Kymene 557 LX based on the dry weight of the ultimately resulting sanitary tissue product.
  • the absorption of the permanent wet strength resin is enhanced by passing the treated slurry through an in-line mixer.
  • aqueous solution of Carboxymethyl cellulose (CMC) dissolved in water and diluted to a solution strength of 1% is added next to the NSK stock pipe after the in-line mixer at a rate of about 0.1% CMC by weight based on the dry weight of the ultimately resulting sanitary tissue product.
  • the aqueous slurry of NSK fibers passes through a centrifugal stock pump to aid in distributing the CMC.
  • An aqueous dispersion of DiTallow DiMethyl Ammonium Methyl Sulfate (DTDMAMS) 77°C (170° F)) at a concentration of 1% by weight is added to the NSK stock pipe at a rate of about 0.1% by weight DTDMAMS based on the dry weight of the ultimately resulting sanitary tissue product.
  • An aqueous slurry of eucalyptus bleached kraft fibrous pulp fibers (from Aracruz - Brazil) of about 1.5% by weight is made up using a conventional repulper and is passed through a stock pipe toward the headbox of the Fourdrinier.
  • This Eucalyptus furnish joins the NSK slurry at the fan pump where both are diluted with white water to about 0.2% consistency.
  • An aqueous slurry of eucalyptus bleached kraft fibrous pulp fibers (from Aracruz - Brazil) of about 3% by weight is made up using a conventional repulper.
  • the Eucalyptus slurry passes to the second fan pump where it is diluted with white water to a consistency of about 0.2%.
  • the slurries of NSK/eucalyptus and eucalyptus are directed into a multi-channeled headbox suitably equipped with layering leaves to maintain the streams as separate layers until discharged onto a traveling Fourdrinier wire.
  • a three-chambered headbox is used.
  • the eucalyptus slurry containing 48% of the dry weight of the ultimate sanitary fibrous structure is directed to the chamber leading to the layer in contact with the wire, while the NSK/eucalyptus slurry comprising 52% (27-35% NSK and 17-25% eucalyptus) of the dry weight of the ultimate paper is directed to the chamber leading to the center and inside layer.
  • the NSK/eucalyptus and eucalyptus slurries are combined at the discharge of the headbox into a composite slurry.
  • the composite slurry is discharged onto the traveling Fourdrinier wire and is dewatered assisted by a deflector and vacuum boxes.
  • the embryonic wet fibrous structure is transferred from the Fourdrinier wire, at a fiber consistency of about 17% by weight at the point of transfer, to a patterned drying fabric.
  • the drying fabric is designed to yield a pattern-densified tissue with discontinuous low-density deflected areas arranged within a continuous network of high density (knuckle) areas.
  • This drying fabric is formed by casting an impervious resin surface onto a fiber mesh supporting fabric.
  • the supporting fabric is a 48 x 52 filament, dual layer mesh.
  • the thickness of the resin cast is about 8 mil above the supporting fabric.
  • the knuckle area is about 35-50% and the open cells remain at a frequency of about 68-562 per square inch.
  • Further de-watering is accomplished by vacuum assisted drainage until the fibrous structure has a fiber consistency of about 23-27%. While remaining in contact with the patterned forming fabric, the patterned fibrous structure is pre-dried by air blown through to a fiber consistency of about 60% by weight. The semi-dry fibrous structure is then adhered to the surface of a Yankee dryer with a sprayed creping adhesive comprising a 0.250% aqueous solution of polyvinyl alcohol. The creping adhesive is delivered to the Yankee surface at a rate of 0.1% adhesive solids based on the dry weight of the fibrous structure. The fiber consistency is increased to about 98% before the fibrous structure is dry creped from the Yankee with a doctor blade.
  • the fibrous structure is calendared across all its width with a steel to rubber calendar roll operating at a loading of 20.7 - 34.5 bar (300-500 psi).
  • the resulting tissue has a basis weight of about 20-25 g/m2; a 1-ply total dry tensile between 250 and 370 g/2.54 cm (250 and 370 g/in), a 1-ply wet burst between 35 and 65 g/2.54cm (35 and 65 gr/in) and a 2-ply caliper of about 0.038 - 0.05 cm (0.015-0.020 inches).
  • the resulting tissue is then combined with a like sheet to form a two-ply, creped, pattern-densified tissue so that the eucalyptus fibers face the outside and it is subjected to calendaring between two smooth steel calendar rolls.
  • the product is then ply-bonded using a mechanical plybond wheel to ensure that both plies stay together.
  • the resulting two-ply tissue has a) a total basis weight of about 39-50 g/m2; b) a 2-ply total dry tensile between 450 and 700 g/2.54 cm (450 and 700 gr/in); c) a 2-ply wet burst between 100 and 130 g/2.54 cm (100 and 130 g/in); d) a 4-ply caliper of about 0.51 and 0.89 mm.
  • fibrous structures described above can be used in combination with any of the treatment processes and lotion compositions described below.
  • the combined parent roll is subsequently converted into a sanitary tissue product.
  • the multi-ply parent roll is unwound and subjected to calandering between two smooth steel calender rolls followed by high pressure embossing to achieve ply bonding.
  • the majority of the fibrous structure remains unaffected by the high pressure embossing.
  • the surface treating composition and the lotion composition are then applied to the fibrous structure as described in detail below.
  • the surface treating composition is printed onto the surface of the 4-ply fibrous structure and/or sanitary tissue product using a roto-gravure printing process. About 1.5 g/m 2 of the surface treatment composition is transferred to each side of the 4-ply product.
  • the printing station consists of two engraved anilox rolls facing each other in a horizontal arrangement and forming a gap in between through which the fibrous structure and/or sanitary tissue product is run.
  • the geometry is arranged in a way that the rolls touch the fibrous structure and/or sanitary tissue product and transfer lotion composition macroscopically uniformly onto both surfaces of the 4-ply fibrous structure and/or sanitary tissue product but the fibrous structure and/or sanitary tissue product does not wrap any of the two anilox rolls.
  • the anilox rolls are engraved to a cell volume of about 3 ml per square meter and about 100 cells per square centimeter, and supplied with lotion composition from a closed supply chamber designed to fill the engraved volume with lotion composition. The gap between the two rolls is adjusted to achieve the target add-on level.
  • Surface coverage of the surface treatment composition was substantially 100% and homogenious. Surface coverage can, e.g. be tested using a surface treatment composition that has 0.01% Tinopal CBS-X added, a fluorescent dye, available from Ciba Speciality Chemicals, Basel, Switzerland.
  • Samples have also been made using an identical application system as described below for the application of lotion composition.
  • the equipment was operated at ambient temperature at a disc speed of about 4000rpm. Surface coverage of this application is lower than using a printing process as described above. While still within the scope of this invention, this process is therefore less preferred.
  • the lotion composition is applied to the fibrous structure and/or sanitary tissue product.
  • the fibrous structure and/or sanitary tissue product span between the two operations was about 5 meter.
  • a commercially available rotary spray application system RFT-Compact-III with applicator heads for the tissue and textile industry (available from Weitmann&Konrad GmbH & Co KG, Leinfelden vomerdingen, Germany) was modified to be used to practice the present invention.
  • the application head is equipped with 5 sets of rotary disks (type 1/1) and has an effective application width of 448mm.
  • the housing of the application head was replaced with water heated walls on the top, the bottom and the rear side of the application head. The whole unit was then insulated towards the outside.
  • Heating units with an integrated pump (Type W60/10-12/40, available from Kelviplast GmbH, Germany) are used to supply the application units with water of the desired temperature.
  • the design of the heating elements was chosen so that the temperature inside the application head is within +/-2°C from the target temperature:
  • the lotion composition infeed of the application heads are connected through a heat traced piping system to a heated pump that is connected through heat traced piping to a heated 100liter tank that holds the melted lotion composition.
  • the return lines of the applicator feed back into the heated tank.
  • a heated flow meter was installed in the lotion composition supply line between pump and application heads.
  • the flow meter (Promass 63M, available from Endress & Hauser, Switzerland) was connected to the control unit of the RFT-Compact-III system that was then used to control the lotion composition pump (Gear pump of type Labu Brox) to deliver the desired lotion composition flow to the application heads.
  • Each set of rotating surfaces consisted of 2 rotating discs stacked on top of each other.
  • the lotion composition supply to the two rotating surfaces of each stack is equally split.
  • the discs have a diameter of about 98mm.
  • the five individual stacks of rotating surfaces are spaced apart by about 112mm.
  • the first, third and fifth set of rotating surfaces is installed vertically shifted versus the second and fourth stack of rotating surfaces to avoid interference between the horizontally overlapping streams of droplets.
  • the sets of rotating surfaces are commercially available from Weitmann & Konrad GmbH & Co, Germany (type 1/1, Art. No. 618996 [upper set] and 618997 [lower set]).
  • the applicator is operated horizontally and with a distance of about 154mm between the fibrous structure and/or sanitary tissue product and the center of the disks.
  • the fibrous structure and/or sanitary tissue product is run vertically from top to bottom between the two application heads.
  • each stack of rotating surfaces covers a cross direction width of about 224mm on the fibrous structure and/or sanitary tissue product with the exception of the two outer stacks of rotating surfaces of the applicator which only cover 112mm each. At each position the streams of two stacks of rotating surfaces are overlapping.
  • the lotion composition temperature is controlled to a determined value through the heating of the tank, the piping and the temperature in the application heads to the desired value.
  • the flow rate is adjusted to achieve the desired add-on level of the fibrous structure.
  • the fibrous structure and/or sanitary tissue product is typically kept at room temperature.
  • the surface area coverage of the lotion composition is about 15% for the sample made with 3g/m 2 lotion application per fibrous structure and/or sanitary tissue product side, a disc speed of about 2500rpm, and a lotion composition temperature in the applicator of about 56°C.
  • the rotating surfaces are operated at 2500rpm for the samples described below but additional samples are made at speeds between 200rpm and 5000rpm.
  • the lotion composition is usually maintained at a temperature of about 5-10°C above the melting point, for the lotion compositions described below all temperature settings are kept at 56°C. Products are made at temperatures less than 2°C below and more than 10°C above the melting point.
  • the fibrous structure and/or sanitary tissue product speed for the examples below is 200m/min, but samples can be made at fibrous structure and/or sanitary tissue speeds between 10m/min and 400m/min.
  • the local surface treating composition and/or lotion composition basis weight on the surface of the fibrous structure can be determined by scanning IR/NIR (infrared or near infrared) spectroscopy in transmission mode (absorption spectroscopy) using a Perkin Elmer Spectrum Spotlight 300 instrument in combination with Spotlight software version 1.1.0 B38.
  • IR/NIR infrared or near infrared
  • the measurements are done with samples representative for the tissue.
  • a 5 x 5 mm sample (or larger) is placed on the sample holder, which is mounted on a XY table and the spectral area used for analysis is scanned at a spatial resolution of 25 ⁇ m in both x and y dimension.
  • the region between 4000cm-1 and 4500cm-1 is scanned and the range between 4296cm-1 (W1) and 4368cm-1 (W2) is used for analysis. At least 16 scans are taken at a resolution of 1 cm-1. If more than 16 scans are used, care needs to be taken that the sample does not change structure as a result of heating up.
  • a map of the local basis weight of the sample is generated.
  • the integrated absorption between W2 and W1 and above a sloping linear baseline is determined for each pixel of 25 ⁇ m x 25 ⁇ m using the ChemiMap menu of the software.
  • the baseline is defined by the absorbency at W1 and W2.
  • the two base points option is chosen in the ChemiMap menu of the software and set at W1 and W2.
  • Start and end point of the integration are also set at W1 and W2.
  • the scaling with the factor DW transforms the average absorbance above the baseline within the wave number range W1 to W2 into an integrated absorption above the baseline.
  • the factor F translates the integrated absorption into local basis weight in g/m 2 .
  • the file which is generated with the ChemiMap command, contains the local basis weight for each pixel of 25 ⁇ m x 25 ⁇ m in area.
  • the file is saved as a text file (.txt format) and also as a bitmap (.bmp format) in 8 bit grey scale format.
  • the text file is imported into EXCEL and the first row and first column are removed (they do not contain image data, but position data).
  • the resulting data are representing the array of pixels of local basis weight in g/m 2 .
  • the maximum (MaxLBW) and minimum (MinLBW) value, as well as the average (AvgLBW) of the whole dataset is calculated in EXCEL.
  • the bitmap file (.bmp file) is imported into AnalySIS image analysis software for further processing (Analysis Pro version 3.1 (build 508), available from Soft Imaging GmbH, Germany).
  • the imported grey scale file is still in RGB format with all three color channels set equal (in 8 bit resolution).
  • AnalySIS the file is color separated to extract one of the three identical color channels (red).
  • the image is calibrated in x-y by setting the pixel size in x and y dimension to match the original sample.
  • the G values can be easily transformed into local basis weight numbers by the following relationship:
  • LLBW can be local lotion composition basis weight or local surface treating composition basis weight depending upon what is being measured.
  • the average value of all local basis weight datapoints above 10g/m 2 can be calculated from the EXCEL datafile.
  • the areas of the composition are defined to have a certain minimum and/or maximum area is set as a filter.
  • the area percentage of composition larger than a certain area is calculated by dividing the area of the composition calculated without area filter, divided by the area of the composition calculated with area filter.
  • the factor F to convert integrated absorption values into local lotion basis weight values is determined by the following procedure: A representative set of calibration samples of known average basis weight of the composition is scanned in the spectral range used for the analysis as described above and analyzed for integrated peak area between W1 and W2 (4296cm-1 and 4368cm-1 for mostly hydrocarbon like materials). The integrated peak area is obtained from the procedure above if the factor F is set equal to 1. The dataset is then imported to EXCEL and the average pixel value of this dataset is calculated. As the factor F was set equal to 1 this value is equal to the mean integrated peak area (AIPA) of the sample in the wave number range W1 to W2.
  • AIPA mean integrated peak area
  • Calibration samples to determine the factor F can either be prepared or an existing composition-containing sample can be used. If an existing sample is used the composition basis weight can be determined by extraction. An example for such a procedure is given below. Examples for how the factor F is determined by analyzing an existing sample (market product) and by preparing calibration samples is also given below. It is important, that the absorbency in the wavelength range used for analysis should never exceed about 1 to ensure a linear correlation between the infrared signal and the local composition basis weight
  • Preparation of calibration samples A suitable piece of the substrate of known area, weight and basis weight is evenly treated with the composition.
  • a suitable type of equipment is a hot wax cartridge spray gun type MK-DUO Line Art.No. 140101, available from MK H exertwachstechnik GmbH, Aichach, Germany.
  • the composition is equilibrated in the sheet by placing the sample in an oven at a temperature of about 10°C above the mp (or at a temperature suitable to allow for sufficient equilibration of the composition in/on the sheet). For relatively low viscosity samples equilibration for about an hour is sufficient. The sample is then cooled down to room temperature and equilibrated for moisture content at 23°C (+-1°C) and 50% (+-2%) relative humidity and weighed again.
  • composition basis weight of that sample [in g/m 2 ] is then calculated as (sample weight after composition treatment [in grams] - sample weight before composition treatment [in grams]) divided by area of the sample [in m 2 ].
  • the samples are then analyzed by the procedure described above to determine the factor F.
  • calibration samples are prepared in a range of composition basis weights that include the range to be measured.
  • Factor F composition basis weight g / m 2 / average integrated peak area
  • composition does not contain a sufficient amount of linear hydrocarbon like material, or the substrate contains materials that do not allow for a quantification of composition between 4296cm-1 and 4368cm-1
  • a different wave number range in the infrared or near infrared range has to be identified that is suitable to quantify the composition by IR spectroscopy. Any wave number range with a linear correlation between integrated absorption coefficient above base line and composition basis weight can be used. If more than one possible wave number range can be identified, the range with the best signal to noise ratio is used. Whenever the composition is based on linear hydrocarbon like materials with CH2 groups the absorption band between 4296cm-1 and 4368cm-1 should be used.
  • Relative concentration of a composition on a surface of the fibrous structure and/or sanitary tissue product may be determined by using near IR spectroscopy, especially if the sample contains a hydrocarbon-containing composition.
  • the near IR spectroscopy method may use a filter photometer or other near IR instrument, but it must be configured for back scatter detection. Appropriate wavelengths are used.
  • the fibrous structure and/or sanitary tissue product is placed under the near IR instrument and a reading is obtained.
  • the sample is then turned over to obtain a reading from the other side of the sample.
  • mid-IR spectroscopy with suitable equipment and wavelengths may also be used to determine relative concentration of a composition on a surface of a fibrous structure and/or sanitary tissue product.

Claims (21)

  1. Structure fibreuse comprenant une surface de contact avec l'utilisateur dans laquelle la surface de contact avec l'utilisateur comprend une première région comprenant une composition de traitement de surface et une deuxième région comprenant une composition de lotion, dans laquelle la première région comprend une composition différente de la composition présente dans la deuxième région et dans laquelle la composition de traitement de surface comprend un agent de traitement de surface choisi dans le groupe constitué de : polymères, hydrocarbures, cires, huiles, silicones, composés d'ammonium quaternaire, fluorocarbures, alcanes substitués en C10 à C22, alcènes substitués en C10 à C22, polyols, dérivés de sucre et leurs mélanges, de préférence dans laquelle les silicones sont choisies dans le groupe constitué de :
    polysiloxanes, aminosilicones, silicones cationiques, silicones quaternaires, bétaïnes de silicone et leurs mélanges, de préférence dans laquelle les polysiloxanes sont choisis parmi des composés ayant des motifs siloxane monomères de structure suivante :
    Figure imgb0010
    dans laquelle, R1 et R2, pour chaque motif monomère siloxane indépendant, peuvent chacun être indépendamment un hydrogène ou n'importe quel radical alkyle, aryle, alcényle, alkaryle, aralkyle, cycloalkyle, hydrocarboné halogéné ou autre radical.
  2. Structure fibreuse selon la revendication 1, dans laquelle la première région comprend un réseau continu ou essentiellement continu et la deuxième région comprend une pluralité de zones distinctes dispersées sur l'ensemble du réseau continu ou essentiellement continu.
  3. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la première région comprend une pluralité de zones distinctes.
  4. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la deuxième région comprend une pluralité de zones distinctes.
  5. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la première région et la deuxième région sont en contact l'une avec l'autre.
  6. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la première région et la deuxième région sont indépendantes et distinctes l'une de l'autre.
  7. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la surface de contact avec l'utilisateur comprend une partie dans laquelle la première région est en contact avec la deuxième région et une autre partie dans laquelle la première région est indépendante et distincte de la deuxième région.
  8. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle au moins la première région est associée à une surface de la structure fibreuse, de préférence dans laquelle la première région est associée à la superficie entière ou la superficie essentiellement entière de la surface de la structure fibreuse, de préférence dans laquelle la composition de traitement de surface de la première région est présente sur la surface de la structure fibreuse à un taux plus grand en poids qu'au sein de la structure fibreuse.
  9. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la deuxième région est associée à une surface de la structure fibreuse.
  10. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la deuxième région est présente sur une surface de la première région de telle sorte que la première région est positionnée entre la deuxième région et une surface de la structure fibreuse, de préférence dans laquelle la deuxième région est présente sur moins de toute la superficie de la surface de la première région, de préférence dans laquelle la deuxième région est présente sur la première région sous la forme d'îles indépendantes, distinctes.
  11. Structure fibreuse selon la revendication 1, dans laquelle les composés d'ammonium quaternaire sont choisis parmi les composés de formule :
    Figure imgb0011
     dans laquelle :
    m est 1 à 3 ; chaque R1 est indépendamment un groupe alkyle en C1 à C6, un groupe hydroxyalkyle, un groupe hydrocarbyle ou hydrocarbyle substitué, un groupe alcoxylé, un groupe benzyle, ou leurs mélanges ; chaque R2 est indépendamment un groupe alkyle en C14 à C22, un groupe hydroxyalkyle, un groupe hydrocarbyle ou hydrocarbyle substitué, un groupe alcoxylé, un groupe benzyle, ou leurs mélanges ; et X- est n'importe quel anion compatible avec un adoucissant.
  12. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la composition de lotion comprend un composé choisi dans le groupe constitué de : hydrocarbures, esters d'acide gras, éthoxylates d'alcool et leurs mélanges.
  13. Structure fibreuse selon l'une quelconque des revendications précédentes, dans laquelle la composition de lotion est une composition de lotion à haute aptitude au transfert susceptible d'être transférée sur une surface opposée.
  14. Utilisation de la structure fibreuse selon l'une quelconque des revendications précédentes dans un produit de papier hygiénique à simple couche ou multicouche.
  15. Structure fibreuse selon la revendication 1, dans laquelle la composition de traitement de surface est présente sur une surface de la structure fibreuse à un taux plus grand en poids qu'au sein de la structure fibreuse et la composition de lotion est présente au sein de la structure fibreuse à un taux plus grand en poids que sur la surface de la structure fibreuse.
  16. Structure fibreuse selon la revendication 15, dans laquelle la composition de lotion est une composition de lotion à haute aptitude au transfert susceptible d'être transférée sur une surface opposée.
  17. Structure fibreuse selon la revendication 15, dans laquelle la composition de lotion est présente sur moins de la superficie entière de la surface de la structure fibreuse.
  18. Structure fibreuse selon la revendication 15, dans laquelle la composition de traitement de surface est présente sur moins de la superficie entière de la surface de la structure fibreuse.
  19. Structure fibreuse selon la revendication 15, dans laquelle la surface de la structure fibreuse comprend des îles indépendantes, distinctes de la composition de lotion.
  20. Structure fibreuse selon la revendication 15, dans laquelle la composition de lotion est présente sur une surface de la composition de traitement de surface.
  21. Utilisation de la structure fibreuse selon l'une quelconque des revendications 15 à 20 dans un produit de papier hygiénique à une seule couche ou multicouche, de préférence dans laquelle le produit de papier hygiénique est un produit de papier hygiénique multicouche et la composition de lotion est présente entre deux ou plusieurs couches du produit de papier hygiénique multicouche.
EP05738715A 2004-04-23 2005-04-09 Structures fibreuses contenant une composition de traitement de surface et une composition de lotion Not-in-force EP1738025B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US56510404P 2004-04-23 2004-04-23
US56510504P 2004-04-23 2004-04-23
US65723005P 2005-02-28 2005-02-28
PCT/US2005/013684 WO2005106119A1 (fr) 2004-04-23 2005-04-09 Structures fibreuses contenant une composition de traitement de surface et une composition de lotion

Publications (2)

Publication Number Publication Date
EP1738025A1 EP1738025A1 (fr) 2007-01-03
EP1738025B1 true EP1738025B1 (fr) 2009-09-30

Family

ID=34966784

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05738715A Not-in-force EP1738025B1 (fr) 2004-04-23 2005-04-09 Structures fibreuses contenant une composition de traitement de surface et une composition de lotion

Country Status (10)

Country Link
EP (1) EP1738025B1 (fr)
JP (1) JP2007534853A (fr)
AT (1) ATE444398T1 (fr)
AU (1) AU2005238469B2 (fr)
CA (1) CA2563539C (fr)
DE (1) DE602005016910D1 (fr)
DK (1) DK1738025T3 (fr)
ES (1) ES2330022T3 (fr)
MX (1) MXPA06012198A (fr)
WO (1) WO2005106119A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070071797A1 (en) * 2005-09-16 2007-03-29 Hernandez-Munoa Diego A Lotioned fibrous structures
JP5394684B2 (ja) * 2008-07-31 2014-01-22 大王製紙株式会社 衛生薄葉紙
US9649830B2 (en) 2008-12-03 2017-05-16 The Procter & Gamble Company Bonded fibrous sanitary tissue products and methods for making same
US20100136294A1 (en) * 2008-12-03 2010-06-03 John Allen Manifold Fibrous structures comprising a lotion and methods for making same
JP5395101B2 (ja) * 2011-02-28 2014-01-22 大王製紙株式会社 トイレットペーパーの製造方法
JP6310493B2 (ja) * 2016-03-31 2018-04-11 大王製紙株式会社 ティシュペーパーの製造方法

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3994771A (en) * 1975-05-30 1976-11-30 The Procter & Gamble Company Process for forming a layered paper web having improved bulk, tactile impression and absorbency and paper thereof
US4300981A (en) * 1979-11-13 1981-11-17 The Procter & Gamble Company Layered paper having a soft and smooth velutinous surface, and method of making such paper
JP2780059B2 (ja) * 1990-04-18 1998-07-23 日本製紙株式会社 ローシヨンペーパー及びその製造方法
JP2001508503A (ja) * 1997-06-17 2001-06-26 ザ、プロクター、エンド、ギャンブル、カンパニー 選択的に配置された化学添加剤を含有するティッシュ・ペーパー
US6179961B1 (en) * 1997-10-08 2001-01-30 The Procter & Gamble Company Tissue paper having a substantive anhydrous softening mixture deposited thereon
US6261580B1 (en) * 1997-10-22 2001-07-17 The Procter & Gamble Company Tissue paper with enhanced lotion transfer
EP1005858A1 (fr) * 1998-12-01 2000-06-07 The Procter & Gamble Company Article en papier tissu et procédé de fabrication de cet article
EP1104821A1 (fr) * 1999-11-26 2001-06-06 The Procter & Gamble Company Papier tissu multicouche épais et lisse
JP2001252214A (ja) * 2000-03-14 2001-09-18 Crecia Corp 薄葉紙ならびにその製法
US6612821B1 (en) * 2000-07-14 2003-09-02 Fluid Management, Inc. Pump, in particular gear pump including ceramic gears and seal
EP1233107B1 (fr) * 2001-02-16 2007-08-22 The Procter & Gamble Company Papier tissue gaufré et traite avec une lotion
EP1749133A1 (fr) * 2004-04-23 2007-02-07 The Procter and Gamble Company Structures fibreuses comprenant un agent pouvant etre transfere

Also Published As

Publication number Publication date
AU2005238469B2 (en) 2008-02-14
MXPA06012198A (es) 2007-01-17
EP1738025A1 (fr) 2007-01-03
DE602005016910D1 (de) 2009-11-12
WO2005106119A1 (fr) 2005-11-10
ES2330022T3 (es) 2009-12-03
CA2563539A1 (fr) 2005-11-10
DK1738025T3 (da) 2010-02-01
AU2005238469A1 (en) 2005-11-10
JP2007534853A (ja) 2007-11-29
ATE444398T1 (de) 2009-10-15
CA2563539C (fr) 2013-08-13

Similar Documents

Publication Publication Date Title
US8557269B2 (en) Paper tissue with high lotion transferability
CA2622804C (fr) Structures fibreuses impregnees
EP0808388B1 (fr) Tissu ouate non crepe traite par sechage a air traversant
US11492758B2 (en) Fibrous structures comprising a surface softening composition
WO2009097231A1 (fr) Papier-tissu doux ayant un composé polyhydroxy et une lotion appliquée sur une surface de celui-ci
EP1738025B1 (fr) Structures fibreuses contenant une composition de traitement de surface et une composition de lotion
CA2516924C (fr) Structure fibreuse et son procede de production
US7229528B2 (en) Processes for foreshortening fibrous structures
AU2005238503B2 (en) Tissue paper with protruding lotion deposits
US20050238699A1 (en) Fibrous structures comprising a surface treating composition and lotion composition
US7758723B2 (en) Processes for foreshortening fibrous structures
AU2004214913B2 (en) Fibrous structure and process for making same

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20061101

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU MC NL PL PT RO SE SI SK TR

17Q First examination report despatched

Effective date: 20070503

DAX Request for extension of the european patent (deleted)
GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU MC NL PL PT RO SE SI SK TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REF Corresponds to:

Ref document number: 602005016910

Country of ref document: DE

Date of ref document: 20091112

Kind code of ref document: P

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2330022

Country of ref document: ES

Kind code of ref document: T3

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

REG Reference to a national code

Ref country code: DK

Ref legal event code: T3

LTIE Lt: invalidation of european patent or patent extension

Effective date: 20090930

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100201

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100130

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DK

Payment date: 20100312

Year of fee payment: 6

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: BE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20100312

Year of fee payment: 6

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20100420

Year of fee payment: 6

Ref country code: FR

Payment date: 20100420

Year of fee payment: 6

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20100430

Year of fee payment: 6

Ref country code: IT

Payment date: 20100423

Year of fee payment: 6

26N No opposition filed

Effective date: 20100701

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20091231

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20100430

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20100409

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20100430

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20100430

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20110409

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20111230

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20111101

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20110502

REG Reference to a national code

Ref country code: DK

Ref legal event code: EBP

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 602005016910

Country of ref document: DE

Effective date: 20111101

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20110409

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20110409

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20120604

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20110430

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20110410

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100401

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20100409

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20090930