US20060185805A1 - Composition for the fluorescent whitening of paper - Google Patents

Composition for the fluorescent whitening of paper Download PDF

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Publication number
US20060185805A1
US20060185805A1 US10/566,742 US56674204A US2006185805A1 US 20060185805 A1 US20060185805 A1 US 20060185805A1 US 56674204 A US56674204 A US 56674204A US 2006185805 A1 US2006185805 A1 US 2006185805A1
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United States
Prior art keywords
paper
alkyl
composition
fluorescent whitening
paperboard
Prior art date
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Abandoned
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US10/566,742
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English (en)
Inventor
Peter Rohringer
Robert Hochberg
Oliver Becherer
Hans Kramer
Goetz Scheffler
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Individual
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Individual
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Publication of US20060185805A1 publication Critical patent/US20060185805A1/en
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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
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/32—Bleaching agents
    • 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
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • 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
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/30—Luminescent or fluorescent substances, e.g. for optical bleaching

Definitions

  • the present invention relates to a composition for the fluorescent whitening of paper, the use thereof in either the pulp mass, in coating or in the metering size-press or film press and to a process thereto.
  • FWA's Traditional fluorescent whitening agents for paper, as disclosed, for example, in DE OS 2,715,864, are derivatives of 4,4′-bis[(1,3,5-triazin-2-yl)amino]stilbene-2,2′-disulphonic acid in which the triazine rings are substituted with anilino residues.
  • these anilino residues may be unsubstituted or substituted by one or two sulphonic acid groups, the resulting FWA's thus being designated as di-, tetra- or hexa-sulphonic acid derivatives.
  • compositions which show both high affinity to the paper and, at the same time, are highly effective in whitening with high saturation points.
  • the present invention relates to a composition for the fluorescent whitening of paper comprising
  • compositions generally comprise
  • component c 0 to 40% by weight of component c), each range being based on the total weight of the composition and wherein the sum of the components a) to c) amounts to 100%.
  • compositions are free flowing liquids and comprise
  • component c 0 to 10% by weight of component c), or 0 to 40% in case polyethylene glycol is used as component c), each range being based on the total weight of the composition and wherein the sum of the components a) to c) amounts to 100%.
  • Component a) of the compositions, the fluorescent whitening agent is a compound of the formula I wherein X 1 , X 2 and X 3 each, independent of the other, represent —NR 1 R 2 or —OR 3 , wherein R 1 and R 2 are, independently of each other, hydrogen, a C 1 -C 4 alkyl-group, which is unsubstituted or substituted by one or two of the following residues selected from the group consisting of C 1 -C 4 alkoxy, hydroxy, carboxy, cyano, carbonamido, thiol, guanidine, substituted or unsubstituted phenyl, unsubstituted or C 1 -C 4 alkyl-substituted C 5 -C 8 cycloalkyl, halogen, a heterocycle and a sulphonic acid residue, and wherein the carbon chain of an alkyl group having two, three or four carbon atoms can be interrupted by oxygen, or, alternatively, R 1 and R
  • component a) is a compound of formula (1), in which X 1 and X 2 each independently, represent —NH 2 , —NHC 1 -C 4 alkyl, —N(C 1 -C 4 alkyl) 2 , —NHC 2 -C 4 hydroxyalkyl, —N(C 2 -C 4 hydroxyalkyl) 2 , —N(C 1 -C 4 alkyl)(C 2 -C 4 hydroxyalkyl), —NH(C 2 -C 4 alkylene-C 1 -C 4 alkoxy), —N(C 1 -C 4 alkylene-C 1 -C 4 alkoxy) 2 , —NHC 1 -C 4 alkylphenyl, tetrahydrofurfurylamino, morpholino, piperidino, pyrrolidino or cyclohexylamino or an amino acid or amino acid amide residue from which a hydrogen atom has been abstracte
  • X 3 represents —NH 2 ,
  • compositions are those in which, in the compound of formula (1),
  • X 1 and X 2 both represent —NH 2 , —NHC 1 -C 2 alkyl, —N(C 1 -C 2 alkyl) 2 , —NHCH 2 CH 2 OH, —N(CH 2 CH 2 OH) 2 , —N(C 1 -C 2 alkyl)(CH 2 CH 2 OH), —NHCH 2 CH 2 OCH 3 , —N(CH 2 CH 2 OCH 3 ) 2 , —NHCH 2 CH 2 —O—CH 2 CH 2 —OH, —N(CH 2 CH 2 O—CH 2 CH 2 —OH 2 , —NHCH 2 CO 2 M′′, —N(CH 3 )CH 2 CO 2 M′′, —NHCH 2 CH 2 CO 2 M′′, —NHCH(CO 2 M′′)CH 2 CH 2 CH 2 NHC( ⁇ NH)NH 2 , tetrahydrofurfurylamino, benzylamino, cyclohexylamino, pyrrol
  • X 3 represents —NH 2
  • M′′ represents H, K, Na, ammonium or ammonium that is mono-, di-, tri- or tetra-substituted by C 1 -C 4 alkyl and/or C 2 -C 4 hydroxyalkyl, especially Na.
  • C 1 -C 4 alkyl groups are, for example, methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl or t-butyl
  • C 1 -C 4 alkoxy groups are, for example, methoxy, ethoxy, n-propoxy, isopropoxy, n-, sec-, iso- or t-butoxy.
  • a C 2 -C 4 alkylene chain may, for example be an ethylene, n-propylene, methyl ethylene, 1- or 2-methylpropylene, n-butylene or ethylethylene residue, whilst C 2 -C 4 hydroxyalkyl may be 2-hydroxyethyl, 2- or 3-hydroxy-n- or isopropyl or hydroxybutyl.
  • halogen is iodine, bromine, chlorine, fluorine or, especially, chlorine
  • C 5 -C 7 cycloalkylamino is cyclopentylamino, cyclohexylamino, cycloheptylamino or, especially, cyclohexylamino.
  • a carbonamido group may be —C( ⁇ O)NH C 1 -C 4 alkyl, —C( ⁇ O)N(C 1 -C 4 alkyl) 2 or, especially, —C( ⁇ O)NH 2 .
  • a heterocyclic residue may be a five-, six- or seven-membered ring having one or two heteroatoms such as oxygen, sulfur or nitrogen, the rest of the skeleton being carbon atoms.
  • Examples are 2- or 3-tetrahydrofurfuryl, 2- or 3-furyl, 2- or 3-thienyl, 2- or 3-pyrrolyl, 2-, 4- or 5-imidazolyl, 2-, 3- or 4-pyridyl, pyrazinyl, 3-isothiazolyl, 3-isoxazolyl or 2- or 3-pyrrolidinyl.
  • amino acid or amino acid amide residue from which a hydrogen atom has been removed may be derived from glycine, alanine, serine, cysteine, phenylalanine, tyrosine (4-hydroxyphenylalanine), diiodotyrosine, tryptophan ( ⁇ -indolylalanine), histidine (( ⁇ -imidazolylalanine), ⁇ -aminobutyric acid, methionine, valine ( ⁇ -aminoisovaleric acid), norvaline, leucine ( ⁇ -aminoisocaproic acid), isoleucine ( ⁇ -aminomethylvaleric acid), norleucine ( ⁇ -amino-n-caproic acid), arginine, omithine ( ⁇ , ⁇ -diaminovaleric acid), lysine ( ⁇ , ⁇ -diaminocaproic acid), aspartic acid (aminosuccinic acid), glutamic acid ( ⁇ -aminoglutaric acid), th
  • a further preferred example of an amino acid from which an amino acid residue R 1 may be derived is iminodiacetic acid or the mono- or diacid amide thereof, whilst a suitable amino acid amide is 2-hydroxyethylaminopropionamide.
  • Suitable optional auxiliaries of the composition, component c), include, for example, anionic or non-ionic dispersants from the class of ethylene oxide adducts with fatty alcohols, higher fatty acids or alkyl phenols or ethylenediamine ethylene oxide-propylene oxide adducts, copolymers of N-vinylpyrrolidone with 3-vinylpropionic acid, polyethylene glycols having an average molecular weight of from 300 to 10,000, water retention aids, including glycols such as ethylene glycol, glycerol or sorbitol, or biocides or further auxiliaries such as urea, lactones or lactams such as N-methylpyrrolidone, and other solubilizing agents such as dimethyl formamide or dimethyl sulphoxide.
  • anionic or non-ionic dispersants from the class of ethylene oxide adducts with fatty alcohols, higher fatty acids or alkyl phenols or ethylenediamine ethylene
  • the present invention further provides a process for the fluorescent whitening of paper or paperboard comprising contacting the substrate with the fluorescent whitening agent composition of the invention.
  • the composition of the invention may be applied to the paper substrate in the pulp mass, in the form of a paper coating composition, or directly in the metering size press or film press.
  • a further aspect of the present invention provides use of the composition of the invention in a process for the fluorescent whitening of a paper surface, comprising contacting the paper surface with a coating composition comprising a white pigment; a binder dispersion; optionally a water-soluble co-binder; and a sufficient amount of a fluorescent whitening agent composition, according to the present invention, to ensure that the treated paper usually contains 0.01 to 1% by weight, based on the white pigment, of a fluorescent whitening agent of formula (1).
  • the white pigment component of the paper coating composition used according to the method of the present invention there are preferred inorganic pigments, e.g., aluminium or magnesium silicates, such as China clay and kaolin and, further, barium sulfate, satin white, titanium dioxide, calcium carbonate (such as chalk, natural or precipitated calcium carbonate) or talcum; as well as white organic pigments.
  • inorganic pigments e.g., aluminium or magnesium silicates, such as China clay and kaolin and, further, barium sulfate, satin white, titanium dioxide, calcium carbonate (such as chalk, natural or precipitated calcium carbonate) or talcum; as well as white organic pigments.
  • the paper coating compositions used according to the method of the present invention may contain, as binder, inter alia, plastics dispersions based on copolymers of butadiene/styrene, acrylonitrile/butadienelstyrene, acrylic acid esters, acrylic acid esterslstyrenelacrylonitrile, ethylenetinyl chloride and ethylenetvinyl acetate; or homopolymers, such as polyvinyl chloride, polyvinylidene chloride, polyethylene and polyvinyl acetate or polyurethanes.
  • plastics dispersions based on copolymers of butadiene/styrene, acrylonitrile/butadienelstyrene, acrylic acid esters, acrylic acid esterslstyrenelacrylonitrile, ethylenetinyl chloride and ethylenetvinyl acetate; or homopolymers, such as polyvinyl chloride, polyvinylidene chloride, polyethylene
  • a preferred binder consists of styrene/butyl acrylate or styrene/butadiene/acrylic acid copolymers or styrene/butadiene rubbers.
  • Other polymer lattices are described, for example, in the following U.S. Pat. Nos. 3,265,654, 3,657,174, 3,547,899 and 3,240,740.
  • the optional water-soluble protective colloid may be, e.g., soya protein, casein, carboxymethylcellulose, natural or modified starch, chitosan or a derivative thereof or, especially, polyvinyl alcohol.
  • the preferred polyvinyl alcohol protective colloid component may have a wide range of saponification levels and molecular weights; e.g. a saponification level ranging from 40 to 100; and an average molecular weight ranging from 10,000 to 100,000 g/mol.
  • the paper coating compositions used according to the method of the present invention preferably contain 1 to 65% by weight of a white pigment.
  • the binder is preferably used in an amount, which is sufficient to make the dry content of polymeric compound up to 1 to 30% by weight, preferably 3 to 25% by weight, of the white pigment.
  • the amount of fluorescent brightener preparation used according to the invention is calculated so that the fluorescent brightener is preferably present in amounts of 0.01 to 2% by weight, more preferably 0.05 to 1% by weight, and especially 0.05 to 0.6% by weight, based on the white pigment.
  • the paper coating composition used in the method according to the invention can be prepared by mixing the components in any desired sequence at temperatures from 10 to 100° C., preferably 20 to 80° C.
  • the components here also include the customary auxiliaries such as binders, co-binders, rheological modifiers, water retention auxiliaries, dispersants, wet strength agents and boosters.
  • auxiliaries are, for example, natural binders, such as starch, casein, protein or gelatin, cellulose ethers, such as carboxyalkylcellulose or hydroxyalkyloellulose, alginic acid, alginates, polyethylene oxide or polyethylene oxide alkyl ethers, copolymers of ethylene oxide and propylene oxide, polyvinyl alcohol, water-soluble condensation products of formaldehyde with urea or melamine, polyphosphates or polyacrylic acid salts.
  • natural binders such as starch, casein, protein or gelatin
  • cellulose ethers such as carboxyalkylcellulose or hydroxyalkyloellulose
  • alginic acid alginates
  • polyethylene oxide or polyethylene oxide alkyl ethers copolymers of ethylene oxide and propylene oxide
  • polyvinyl alcohol water-soluble condensation products of formaldehyde with urea or melamine
  • polyphosphates or polyacrylic acid salts such as sodium binders,
  • the coating composition used according to the method of the present invention is preferably used to produce coated printed or writing paper, or special papers such as ink-jet or photographic papers, or cardboard.
  • the coating composition used according to the method of the invention can be applied to the substrate by any conventional process, for example with an air blade, a coating blade, a roller, a doctor blade or a rod, in the size press, a metering size press, or by spraying, after which the coatings are dried at a temperature in the range from 70 to 200° C., preferably 90 to 130° C., to a residual moisture content of 3 to 8%, for example with infra-red driers and/or hot-air driers.
  • the present invention provides a method for the fluorescent whitening of a paper surface comprising contacting the paper in the size press or metering size press with an aqueous solution containing a size, optionally an inorganic or organic pigment and 0.1 to 20 g/l of a fluorescent whitening agent composition of the invention.
  • the size is starch, a starch derivative or a synthetic sizing agent, especially a water-soluble copolymer or mixtures thereof.
  • the invention provides a method for the fluorescent whitening of paper during paper formation, whereby the FWA composition is added directly to the pulp mass.
  • the FWA composition may be in the form of a solution or a dispersion, whereby the FWA compositions of the invention are especially valuable in that their effect is only slightly inhibited by the presence of cationic polymers, fixing agents, wet-strengthening agents or de-inking auxiliaries, which are similarly added to the pulp mass prior to paper formation.
  • auxiliaries may include dicyandiamide condensation products, polyvinyl amines, polyethylene imines, cationic starches, poly-DADMAC (diallyl dimethyl ammonium chloride), polyamide amines and polyepoxides.
  • Another embodiment of the present invention relates to paper, which has been treated with a fluorescent whitening agent composition according to the invention.
  • compositions of the invention may be obtained by mechanical mixing of the individual components a), b) and, optionally, c) at ambient or elevated temperature until homogenous solutions or dispersions are obtained.
  • the fluorescent whitening agents, components a), of the invention are known compounds or may be obtained in analogy to known methods as described, for example, in GB 1,183,854.
  • compositions of the present invention are particularly advantageous in that they exhibit not only extremely high whitening ability, but, in addition, in many cases highly desirable water solubilities and fastness properties.
  • the coatings obtained are distinguished by optimum distribution of the fluorescent brightener over the entire surface and by an increase in the level of whiteness thereby achieved, by a high fastness to light and to elevated temperature (e.g. stability for 24 hours at 60 to 100° C.) and excellent bleed-fastness to water.
  • the resulting composition is then applied in a size-press to a neutral-sized, wood- and FWA-free paper having a basis weight of 80 g/m 2 with an uptake of 20% of the composition, based on the weight of the paper.
  • the degrees of whiteness, Wcie, are then measured using a Datacolor Elrepho 3000 spectrophotometer.
  • the corresponding values, Wcie, for the conventional FWA, of the formula are 109 and 110, respectively, thus demonstrating significant improvement in both saturation point and degree of whiteness of the majority of the instant compositions.

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  • Paper (AREA)
  • Luminescent Compositions (AREA)
  • Detergent Compositions (AREA)
US10/566,742 2003-08-06 2004-07-28 Composition for the fluorescent whitening of paper Abandoned US20060185805A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP03102449 2003-08-06
EP03102449.0 2003-08-06
PCT/EP2004/051630 WO2005014932A1 (en) 2003-08-06 2004-07-28 Composition for the fluorescent whitening of paper

Publications (1)

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US20060185805A1 true US20060185805A1 (en) 2006-08-24

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Country Status (15)

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US (1) US20060185805A1 (ko)
EP (1) EP1651816A1 (ko)
JP (1) JP2007501336A (ko)
KR (1) KR20060073588A (ko)
CN (1) CN1833072A (ko)
AR (1) AR045215A1 (ko)
AU (1) AU2004263674A1 (ko)
BR (1) BRPI0413352A (ko)
CA (1) CA2533364A1 (ko)
IL (1) IL173135A0 (ko)
MX (1) MXPA06001366A (ko)
RU (1) RU2006106728A (ko)
TW (1) TW200516193A (ko)
WO (1) WO2005014932A1 (ko)
ZA (1) ZA200600465B (ko)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090106916A1 (en) * 2006-05-23 2009-04-30 Oliver Becherer Detergent Composition for Textile Fibre Materials
US20090146927A1 (en) * 2007-12-06 2009-06-11 Tpo Displays Corp. Method for manufacturing thin film transistor (tft) and oled display having tfts manufactured by the same
US20110263836A1 (en) * 2008-04-22 2011-10-27 Kemira Oyj Method for reduction of light-induced yellowing of lignin-containing material

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2495973C2 (ru) * 2008-03-26 2013-10-20 Клариант Финанс (Бви) Лимитед Усовершенствованные композиции для оптического отбеливания
US20120118522A1 (en) * 2009-07-24 2012-05-17 Clariant Finance (Bvi) Limited Aqueous Solutions Of Acid Dyes For Shading In Size Press Applications

Citations (9)

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US4364845A (en) * 1978-07-17 1982-12-21 Ciba-Geigy Corporation Concentrated aqueous solutions of sulfo group-containing fluorescent brighteners which are stable on storage
US5622749A (en) * 1993-05-08 1997-04-22 Ciba-Geigy Corporation Fluorescent whitening of paper
US5846382A (en) * 1992-09-14 1998-12-08 Jorax Gmbh Process for enhancing the whiteness, brightness and chromaticity of fillers and pigments
US5902454A (en) * 1996-12-13 1999-05-11 Ciba Specialty Chemicals Corporation Method of whitening lignin-containing paper pulps
US5976410A (en) * 1996-10-10 1999-11-02 Ciba Specialty Chemicals Corporation Dispersions of fluorescent whitening agents
US6143888A (en) * 1996-06-04 2000-11-07 Ciba Specialty Chemicals Corporation Use of triazine-based UVAs for use as quenchers in paper-making processes
US6302999B1 (en) * 1997-09-16 2001-10-16 Ciba Specialty Chemicals Corp. Method for optically brightening paper
US20030054969A1 (en) * 2001-04-27 2003-03-20 Eugenio Fumagalli Detergent compositions
US6797752B1 (en) * 1999-08-05 2004-09-28 Ciba Specialty Chemicals Corporation Use of whitening pigments for whitening paper coating compositions

Family Cites Families (3)

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GB1183854A (en) * 1967-07-14 1970-03-11 Bayer Ag Brightening Agents of the Bistriazinylaminostilbene Series
DE2715864A1 (de) * 1976-04-14 1977-10-27 Ciba Geigy Ag Verfahren zum optischen aufhellen von papier
EP0905317B1 (en) * 1997-09-16 2009-12-23 Basf Se A method for optically brightening paper

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4364845A (en) * 1978-07-17 1982-12-21 Ciba-Geigy Corporation Concentrated aqueous solutions of sulfo group-containing fluorescent brighteners which are stable on storage
US5846382A (en) * 1992-09-14 1998-12-08 Jorax Gmbh Process for enhancing the whiteness, brightness and chromaticity of fillers and pigments
US5622749A (en) * 1993-05-08 1997-04-22 Ciba-Geigy Corporation Fluorescent whitening of paper
US6143888A (en) * 1996-06-04 2000-11-07 Ciba Specialty Chemicals Corporation Use of triazine-based UVAs for use as quenchers in paper-making processes
US5976410A (en) * 1996-10-10 1999-11-02 Ciba Specialty Chemicals Corporation Dispersions of fluorescent whitening agents
US5902454A (en) * 1996-12-13 1999-05-11 Ciba Specialty Chemicals Corporation Method of whitening lignin-containing paper pulps
US6302999B1 (en) * 1997-09-16 2001-10-16 Ciba Specialty Chemicals Corp. Method for optically brightening paper
US20020084049A1 (en) * 1997-09-16 2002-07-04 Thomas Engelhardt Method for optically brightening paper
US6464832B2 (en) * 1997-09-16 2002-10-15 Ciba Specialty Chemicals Corporation Method for optically brightening paper
US6797752B1 (en) * 1999-08-05 2004-09-28 Ciba Specialty Chemicals Corporation Use of whitening pigments for whitening paper coating compositions
US20030054969A1 (en) * 2001-04-27 2003-03-20 Eugenio Fumagalli Detergent compositions

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090106916A1 (en) * 2006-05-23 2009-04-30 Oliver Becherer Detergent Composition for Textile Fibre Materials
US8080510B2 (en) 2006-05-23 2011-12-20 Basf Se Detergent composition for textile fibre materials
US20090146927A1 (en) * 2007-12-06 2009-06-11 Tpo Displays Corp. Method for manufacturing thin film transistor (tft) and oled display having tfts manufactured by the same
US20110263836A1 (en) * 2008-04-22 2011-10-27 Kemira Oyj Method for reduction of light-induced yellowing of lignin-containing material

Also Published As

Publication number Publication date
ZA200600465B (en) 2007-03-28
AU2004263674A1 (en) 2005-02-17
JP2007501336A (ja) 2007-01-25
CA2533364A1 (en) 2005-02-17
RU2006106728A (ru) 2007-10-10
MXPA06001366A (es) 2006-05-15
CN1833072A (zh) 2006-09-13
KR20060073588A (ko) 2006-06-28
AR045215A1 (es) 2005-10-19
IL173135A0 (en) 2006-06-11
BRPI0413352A (pt) 2006-10-10
WO2005014932A1 (en) 2005-02-17
TW200516193A (en) 2005-05-16
EP1651816A1 (en) 2006-05-03

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