EP1527155B2 - Waschmittelzusammensetzungen - Google Patents

Waschmittelzusammensetzungen Download PDF

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Publication number
EP1527155B2
EP1527155B2 EP03792209A EP03792209A EP1527155B2 EP 1527155 B2 EP1527155 B2 EP 1527155B2 EP 03792209 A EP03792209 A EP 03792209A EP 03792209 A EP03792209 A EP 03792209A EP 1527155 B2 EP1527155 B2 EP 1527155B2
Authority
EP
European Patent Office
Prior art keywords
polyvinyl pyrrolidone
sodium
detergent composition
pvp
laundry detergent
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.)
Expired - Lifetime
Application number
EP03792209A
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English (en)
French (fr)
Other versions
EP1527155A1 (de
EP1527155B1 (de
Inventor
Donna Unilever R & D Port Sunlight MACNAB
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.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
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Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Publication of EP1527155A1 publication Critical patent/EP1527155A1/de
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Publication of EP1527155B2 publication Critical patent/EP1527155B2/de
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3769—(Co)polymerised monomers containing nitrogen, e.g. carbonamides, nitriles or amines
    • C11D3/3776—Heterocyclic compounds, e.g. lactam
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds

Definitions

  • the present invention relates to laundry detergent compositions containing polyvinyl pyrrolidone.
  • the compositions exhibit improved detergency on oily soils.
  • Polyvinyl pyrrolidone and some related polymers are known ingredients of laundry detergent compositions, providing the benefit of reduced dye transfer between fabrics in a mixed load.
  • Laundry detergent compositions containing polyvinyl pyrrolidone as a dye transfer inhibitor are disclosed, for example, in WO 92 18597A , WO 94 03567A , WO 95 03390A , WO 95 17496A , WO 95 27028A and WO 95 34627A (Procter & Gamble), and WO 94 24249A and WO 97 03166A (Henkel).
  • GB 1 354 498 discloses laundry detergent compositions containing vinyl pyrrolidone/vinyl acetate copolymers as antiredeposition agents. Polyvinyl pyrrolidone itself is stated to be ineffective.
  • EP 0 262 897 discloses a detergent composition
  • a detergent composition comprising an anionic detergent active material, and polyvinyl pyrrolidone further comprising a nonionic material or a mixture there of the nonionic material or its mixture having an HLB of not more than 10.5.
  • polyvinyl pyrrolidone is also effective to enhance oily soil detergency, especially in detergent compositions containing anionic surfactants, more especially alkylbenzene sulphonate.
  • the present invention provides the use of polyvinyl pyrrolidone in a laundry detergent composition according to claim 1 to improve the oily soil detergency of the composition.
  • the polyvinyl pyrrolidone (hereinafter PVP) preferably has a molecular weight within the range of from 10 000 to 100 000, more preferably from 25 000 to 75 000.
  • PVP is commercially available, for example, from BASF as the Luviskol (Trade Mark) K series (powders and solutions of various concentrations) and Sokalan (Trade Mark) HP50 (powder), and from International Specialty Products (ISP) as the ISP-K series.
  • the laundry detergent composition is a laundry detergent composition
  • the PVP is present in an amount sufficient to enhance oily soil detergency.
  • the PVP is present in an amount of from from 0.5 to 3 wt%, preferably from 1 to 2 wt%.
  • the detergent composition may suitably comprise:
  • the organic surfactant is the organic surfactant
  • the detergent composition in accordance with the invention may contain any organic surfactants (detergent-active compounds) suitable for incorporation into laundry detergent compositions.
  • the composition comprises linear alkylbenzene sulphonate (LAS).
  • Detergent-active compounds may be chosen from soap and non-soap anionic, cationic, nonionic, amphoteric and zwitterionic detergent-active compounds, and mixtures thereof.
  • Many suitable detergent-active compounds are available and are fully described in the literature, for example, in "Surface-Active Agents and Detergents", Volumes I and II, by Schwartz, Perry and Berch.
  • the preferred detergent-active compounds that can be used are soaps and synthetic non-soap anionic and nonionic compounds.
  • the total amount of surfactant present is suitably within the range of from 5 to 60 wt%, preferably from 5 to 40 wt%.
  • Anionic surfactants are well-known to those skilled in the art.
  • alkylbenzene sulphonates particularly linear alkylbenzene sulphonates having an alkyl chain length of C 8 -C 15 ; primary and secondary alkylsulphates, particularly C 8 -C 20 primary alkyl sulphates; alkyl ether sulphates; olefin sulphonates; alkyl xylene sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates.
  • Sodium salts are generally preferred.
  • Nonionic surfactants that may be used include the primary and secondary alcohol ethoxylates, especially the C 8 -C 20 aliphatic alcohols ethoxylated with an average of from 1 to 20 moles of ethylene oxide per mole of alcohol, and more especially the C 10 -C 15 primary and secondary aliphatic alcohols ethoxylated with an average of from 1 to 10 moles of ethylene oxide per mole of alcohol.
  • Non-ethoxylated nonionic surfactants include alkylpolyglycosides, glycerol monoethers, and polyhydroxyamides (glucamide).
  • Cationic surfactants that may be used include quaternary ammonium salts of the general formula R 1 R 2 R 3 R 4 N + X - wherein the R groups are long or short hydrocarbyl chains, typically alkyl, hydroxyalkyl or ethoxylated alkyl groups, and X is a solubilising anion (for example, compounds in which R 1 is a C 8 -C 22 alkyl group, preferably a C 8 -C 10 or C 12 -C 14 alkyl group, R 2 is a methyl group, and R 3 and R 4 , which may be the same or different, are methyl or hydroxyethyl groups); and cationic esters (for example, choline esters).
  • R 1 is a C 8 -C 22 alkyl group, preferably a C 8 -C 10 or C 12 -C 14 alkyl group
  • R 2 is a methyl group
  • R 3 and R 4 which may be the same or different, are methyl or
  • Amphoteric surfactants and/or zwitterionic surfactants may also be present.
  • Preferred amphoteric surfactants are amine oxides. These are materials of the general formula R 1 R 2 R 3 N ⁇ O wherein R 1 is typically a C 8 -C 18 alkyl group, for example, C 12 -C 14 alkyl, and R 2 and R 3 , which may be the same or different, are C 1 -C 3 alkyl or hydroxyalkyl groups, for example, methyl groups.
  • the most preferred amine oxide is coco dimethylamine oxide.
  • Preferred zwitterionic surfactants are betaines, and especially amidobetaines.
  • Preferred betaines are C 8 -C 18 alkyl amidoalkylbetaines, for example, coco amidopropyl betaine (CAPB).
  • the compositions contains from 3 to 30 wt%, more preferably from 10 to 25 wt%, of LAS.
  • the detergent compositions in accordance with the invention also contain one or more detergency builders.
  • the detergency builder which is present in an amount of from 10 to 60 wt%, is selected from sodium tripolyphosphate, zeolites, sodium carbonate and mixtures thereof.
  • Preferred builders are alkali metal aluminosilicates, more especially crystalline alkali metal aluminosilicates (zeolites), preferably in sodium salt form.
  • zeolites crystalline alkali metal aluminosilicates
  • Zeolite builders may suitably be present in a total amount of from 5 to 60 wt%, preferably from 10 to 50 wt%.
  • the zeolites may be supplemented by other inorganic builders, for example, amorphous aluminosilicates, or layered silicates such as SKS-6 ex Clariant.
  • the zeolites may be supplemented by organic builders, for example, polycarboxylate polymers such as polyacrylates and acrylic/maleic copolymers; monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyliminodiacetates, alkyl- and alkenylmalonates and succinates; and sulphonated fatty acid salts.
  • polycarboxylate polymers such as polyacrylates and acrylic/maleic copolymers
  • monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyliminodiacetates, alkyl- and
  • compositions in accordance with the invention may contain phosphate builders, for example, sodium tripolyphosphate.
  • phosphate builders for example, sodium tripolyphosphate.
  • organic builders are citrates, suitably used in amounts of from 1 to 30 wt%, preferably from 2 to 15 wt%; and acrylic polymers, more especially acrylic/maleic copolymers, suitably used in amounts of from 0.5 to 15 wt%, preferably from 1 to 10 wt%.
  • Builders, both inorganic and organic, are preferably present in alkali metal salt, especially sodium salt, form.
  • Detergent compositions in accordance with the invention may also suitably contain a bleach system.
  • a bleach system Preferably this will include a peroxy bleach compound, for example, an inorganic persalt or an organic peroxyacid, capable of yielding hydrogen peroxide in aqueous solution.
  • Preferred inorganic persalts are sodium perborate monohydrate and tetrahydrate, and sodium percarbonate, the latter being especially preferred.
  • the sodium percarbonate may have a protective coating against destabilisation by moisture.
  • the peroxy bleach compound is suitably present in an amount of from 5 to 35 wt%, preferably from 10 to 25 wt%.
  • the peroxy bleach compound may be used in conjunction with a bleach activator (bleach precursor) to improve bleaching action at low wash temperatures.
  • the bleach precursor is suitably present in an amount of from 1 to 8 wt%, preferably from 2 to 5 wt%.
  • Preferred bleach precursors are peroxycarboxylic acid precursors, more especially peracetic acid precursors and peroxybenzoic acid precursors; and peroxycarbonic acid precursors.
  • An especially preferred bleach precursor suitable for use in the present invention is N,N,N',N'-tetracetyl ethylenediamine (TAED).
  • a bleach stabiliser may also be present.
  • Suitable bleach stabilisers include ethylenediamine tetraacetate (EDTA), diethylenetriamine pentaacetate (DTPA), ethylenediamine disuccinate (EDDS), and the polyphosphonates such as the Dequests (Trade Mark), ethylenediamine tetramethylene phosphonate (EDTMP) and diethylenetriamine pentamethylene phosphate (DETPMP).
  • compositions in accordance with the invention may contain alkali metal, preferably sodium, carbonate, in order to increase detergency and ease processing.
  • Sodium carbonate may suitably be present in amounts ranging from 1 to 60 wt%, preferably from 2 to 40 wt%.
  • sodium silicate may also be present.
  • the amount of sodium silicate may suitably range from 0.1 to 5 wt%.
  • Sodium silicate, as previously indicated, is preferably introduced via the second base granule.
  • Powder flow may be improved by the incorporation of a small amount of a powder structurant.
  • powder structurants include, for example, fatty acids (or fatty acid soaps), sugars, acrylate or acrylate/maleate polymers, sodium silicate, and dicarboxylic acids (for example, Sokalan (Trade Mark) DCS ex BASF).
  • fatty acids or fatty acid soaps
  • sugars acrylate or acrylate/maleate polymers
  • sodium silicate for example, Sokalan (Trade Mark) DCS ex BASF
  • dicarboxylic acids for example, Sokalan (Trade Mark) DCS ex BASF.
  • One preferred powder structurant is fatty acid soap, suitably present in an amount of from 1 to 5 wt%.
  • antiredeposition agents such as cellulosic polymers; soil release agents; anti-dye-transfer agents; fluorescers; inorganic salts such as sodium sulphate; enzymes (proteases, lipases, amylases, cellulases); dyes; coloured speckles; perfumes; and fabric conditioning compounds. This list is not intended to be exhaustive.
  • compositions in accordance with the invention may be of any suitable physical form, for example, particulates (powders, granules, tablets), liquids, pastes, gels or bars.
  • the detergent composition is in particulate form.
  • Powders of low to moderate bulk density may be prepared by spray-drying a slurry, and optionally postdosing (dry-mixing) further ingredients.
  • “Concentrated” or “compact” powders may be prepared by mixing and granulating processes, for example, using a high-speed mixer/granulator, or other non-tower processes.
  • Tablets may be prepared by compacting powders, especially "concentrated” powders.
  • liquid detergent compositions which may be prepared by admixing the essential and optional ingredients in any desired order to provide compositions containing the ingredients in the requisite concentrations.
  • the PVP may be incorporated at any suitable stage in the manufacture of the compositions in accordance with the invention.
  • PVP is commercially available both in solution form and in solid form.
  • PVP in powder or solution preferably aqueous
  • PVP powder or solution may be easily introduced into mixing and granulating apparatus, either alone or in admixture with other solid or liquid ingredients as appropriate.
  • wash liquors containing 1 g/litre or 2.5 g/litre of a notional detergent composition (the "product") containing linear alkylbenzene sulphonate (LAS) and sodium carbonate were prepared to the following general formulation: Ingredient Weight% in "product" Weight% in 1 g/l wash liquor Weight% in 2.5 g/l wash liquor Sodium LAS 14.82 0.1482 0.3705 Sodium carbonate 11.50 0.1150 0.2785 PVP 0, 0.20 or 0.80 0, 0.0020 or 0.0080 0, 0.0050 or 0.0200 Water Balance Balance Balance Balance Balance Balance Balance
  • Detergency on white cotton cloth soiled with dirty motor oil was assessed using a high throughput small scale wash method.
  • the wash was carried out in water of 20° (French) hardness (Ca:Mg 2:1), at a temperature of 20°C for 20 minutes.
  • Whiteness before and after the wash was determined using the technique of colour change by image analysis using a greyness scale.
  • the results are analogous to reflectance changes at 460 nm as measured by a reflectance spectrophotometer and are expressed as ⁇ R and ⁇ R.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)

Claims (5)

  1. Verwendung von Polyvinylpyrrolidon in einer Wäschewaschmittelzusammensetzung, umfassend lineares Alkylbenzolsulfonat und 10 bis 60 Gew.-% Waschmittelbuilder ausgewählt aus Natriumtripolyphosphat, Zeolithen, Natriumcarbonat und Gemischen davon, um die Waschkraft der Zusammensetzung für öligen Schmutz zu verbessern.
  2. Verwendung nach einem vorangehenden Anspruch, dadurch gekennzeichnet, dass das Polyvinylpyrrolidon ein Molekulargewicht im Bereich von 10 000 bis 100 000, vorzugsweise 25 000 bis 75 000, aufweist.
  3. Verwendung nach einem vorangehenden Anspruch, dadurch gekennzeichnet, dass die Wäschewaschmittelzusammensetzung 0,5 bis 3 Gewichtsprozent, vorzugsweise 1 bis 2 Gewichtsprozent, Polyvinylpyrrolidon enthält.
  4. Verwendung nach einem vorangehenden Anspruch, dadurch gekennzeichnet, dass die Wäschewaschmittelzusammensetzung umfasst:
    (a) 5 bis 60 Gew.-%, vorzugsweise 10 bis 40 Gew.-%, organisches Tensid,
    (b) gegebenenfalls 5 bis 80 Gew.-%, vorzugsweise 10 bis 60 Gew.-%, Waschmittelbuilder,
    (c) 0,5 bis 3 Gew.-%, vorzugsweise 1 bis 2 Gew.-%, Polyvinylpyrrolidon,
    (d) gegebenenfalls andere Waschmittelbestandteile auf 100 Gewichtsprozent.
  5. Verwendung nach einem vorangehenden Anspruch, dadurch gekennzeichnet, dass die Wäschewaschmittelzusammensetzung 3 bis 30 Gew.-%, vorzugsweise 10 bis 25 Gew.-% lineares Alkylbenzolsulfonat enthält.
EP03792209A 2002-08-10 2003-07-16 Waschmittelzusammensetzungen Expired - Lifetime EP1527155B2 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GBGB0218634.4A GB0218634D0 (en) 2002-08-10 2002-08-10 Detergent compositions
GB0218634 2002-08-10
PCT/EP2003/007754 WO2004018603A1 (en) 2002-08-10 2003-07-16 Detergent compositions

Publications (3)

Publication Number Publication Date
EP1527155A1 EP1527155A1 (de) 2005-05-04
EP1527155B1 EP1527155B1 (de) 2006-06-07
EP1527155B2 true EP1527155B2 (de) 2011-04-13

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ID=9942091

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EP03792209A Expired - Lifetime EP1527155B2 (de) 2002-08-10 2003-07-16 Waschmittelzusammensetzungen

Country Status (8)

Country Link
EP (1) EP1527155B2 (de)
AR (1) AR040832A1 (de)
AT (1) ATE328992T1 (de)
AU (1) AU2003246709A1 (de)
BR (1) BR0312731A (de)
DE (1) DE60305927T2 (de)
GB (1) GB0218634D0 (de)
WO (1) WO2004018603A1 (de)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007061861A1 (de) 2007-12-19 2009-06-25 Henkel Ag & Co. Kgaa Wasch- oder Reinigungsmittel mit verbesserter Reinigungsleistung
DE102011112777A1 (de) * 2011-09-09 2013-03-14 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Die Primärwaschkraft verbessernde polymere Wirkstoffe

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3000830A (en) † 1952-12-05 1961-09-19 Fong Willie Use of polyvinylpyrrolidone as a soil-suspending agent
EP0087914A1 (de) † 1982-03-01 1983-09-07 The Procter & Gamble Company Detergenszusammensetzung
GB2137221A (en) † 1983-03-29 1984-10-03 Colgate Palmolive Co Soil releasing detergent
US4954292A (en) † 1986-10-01 1990-09-04 Lever Brothers Co. Detergent composition containing PVP and process of using same
EP0781838A1 (de) † 1995-12-29 1997-07-02 Colgate-Palmolive Company Waschmittelzusammensetzung mit verbesserter Reinigungsleistung
EP0887360A1 (de) † 1997-06-27 1998-12-30 Basf Aktiengesellschaft Verfahren zur Herstellung von niedermolekularen Homopolymerisaten des N-Vinylpyrrolidons
WO1999040168A1 (en) † 1998-02-06 1999-08-12 Precision Fabrics Group, Inc. Laundry detergent compositions containing silica for laundry detergent sheets
WO2001059048A1 (en) † 2000-02-07 2001-08-16 Unilever Plc Detergent compositions
EP1167500A1 (de) † 2000-06-29 2002-01-02 The Procter & Gamble Company Verfahren zum Reinigen einer harten Oberfläche

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Publication number Priority date Publication date Assignee Title
US3318816A (en) * 1964-11-12 1967-05-09 Colgate Palmolive Co Detergent composition in solid form containing a synergistic mixture of cmc and pvp
DE3840056A1 (de) * 1988-11-28 1990-05-31 Henkel Kgaa Verfahren zum waschen von verfaerbungsempfindlichen textilien
US5466802A (en) * 1993-11-10 1995-11-14 The Procter & Gamble Company Detergent compositions which provide dye transfer inhibition benefits
CN1146779A (zh) * 1994-03-04 1997-04-02 普罗格特-甘布尔公司 在织物洗涤中提供染料转移抑制作用的多羟基酰胺
GB9526181D0 (en) * 1995-12-21 1996-02-21 Unilever Plc A detergent composition
EP0985065A4 (de) * 1997-05-28 2001-05-02 Robert H Black Verfahren zur reinigung verschmutzter textilien
JP2001508493A (ja) * 1998-01-13 2001-06-26 ザ、プロクター、エンド、ギャンブル、カンパニー 改善された溶解性を有する洗剤顆粒

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3000830A (en) † 1952-12-05 1961-09-19 Fong Willie Use of polyvinylpyrrolidone as a soil-suspending agent
EP0087914A1 (de) † 1982-03-01 1983-09-07 The Procter & Gamble Company Detergenszusammensetzung
GB2137221A (en) † 1983-03-29 1984-10-03 Colgate Palmolive Co Soil releasing detergent
US4954292A (en) † 1986-10-01 1990-09-04 Lever Brothers Co. Detergent composition containing PVP and process of using same
EP0781838A1 (de) † 1995-12-29 1997-07-02 Colgate-Palmolive Company Waschmittelzusammensetzung mit verbesserter Reinigungsleistung
EP0887360A1 (de) † 1997-06-27 1998-12-30 Basf Aktiengesellschaft Verfahren zur Herstellung von niedermolekularen Homopolymerisaten des N-Vinylpyrrolidons
WO1999040168A1 (en) † 1998-02-06 1999-08-12 Precision Fabrics Group, Inc. Laundry detergent compositions containing silica for laundry detergent sheets
WO2001059048A1 (en) † 2000-02-07 2001-08-16 Unilever Plc Detergent compositions
EP1167500A1 (de) † 2000-06-29 2002-01-02 The Procter & Gamble Company Verfahren zum Reinigen einer harten Oberfläche

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
CUTLER W.G.; DAVIES R.C.: "Detergency: Theory and Test Methods", SURFACTANT SCIENCE SERIES, vol. 5, 1972, MARCEL DEKKER INC., NEW YORK, pages 1 AND 8 - 9 †
NAGARAJAN R.: "Polymer-Surfactant Interactions", NEW HORIZONS: DETERGENTS FOR THE NEW MILLENIUM CONFERENCE INVITED PAPERS, 2001, AMERICAN OIL CHEMISTS SOCIETY AND CONSUMER SPECIALTY PRODUCTS ASSOCIATION, FORT MYERS, FLORIDA †
Technical information ex. BASF on Sokalan HP50 and HP53, May 1991 †
TOKIWA F.; IMAMURA T.: "Detergent Building Action of Uncharged Polymers in relation to their Molecular Weights", JOURNAL OF THE AMERICAN OIL CHEMISTS' SOCIETY, vol. 49, March 1972 (1972-03-01), pages 166 - 169 †
W. GALE CUTLER; ERIK KISSA: "Detergency: theory and technology", SURFACTANT SCIENCE SERIES, vol. 20, 1987, MARCEL DEKKER INC., pages 257 - 260 †

Also Published As

Publication number Publication date
AU2003246709A1 (en) 2004-03-11
WO2004018603A1 (en) 2004-03-04
BR0312731A (pt) 2005-04-19
AR040832A1 (es) 2005-04-20
ATE328992T1 (de) 2006-06-15
EP1527155A1 (de) 2005-05-04
EP1527155B1 (de) 2006-06-07
DE60305927D1 (de) 2006-07-20
GB0218634D0 (en) 2002-09-18
DE60305927T2 (de) 2007-06-06

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