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WO1999013041A1 - Savon solide transparent et pate de savon transparente - Google Patents

Savon solide transparent et pate de savon transparente Download PDF

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Publication number
WO1999013041A1
WO1999013041A1 PCT/JP1997/003137 JP9703137W WO9913041A1 WO 1999013041 A1 WO1999013041 A1 WO 1999013041A1 JP 9703137 W JP9703137 W JP 9703137W WO 9913041 A1 WO9913041 A1 WO 9913041A1
Authority
WO
WIPO (PCT)
Prior art keywords
transparent
stone
fatty acid
organic amine
sodium hydroxide
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.)
Ceased
Application number
PCT/JP1997/003137
Other languages
English (en)
Japanese (ja)
Inventor
Isao Shimosato
Masanori Okada
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.)
Pola Orbis Holdings Inc
Original Assignee
Pola Chemical Industries Inc
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
Priority claimed from JP12728396A external-priority patent/JP3378725B2/ja
Priority to JP12728396A priority Critical patent/JP3378725B2/ja
Priority to BR9712732-9A priority patent/BR9712732A/pt
Priority to CA002270381A priority patent/CA2270381A1/fr
Priority to EP97939200A priority patent/EP0947579B1/fr
Priority to AU41358/97A priority patent/AU720810B2/en
Application filed by Pola Chemical Industries Inc filed Critical Pola Chemical Industries Inc
Priority to US09/297,593 priority patent/US6156714A/en
Priority to NZ335346A priority patent/NZ335346A/en
Priority to DE69736071T priority patent/DE69736071T2/de
Priority to PCT/JP1997/003137 priority patent/WO1999013041A1/fr
Publication of WO1999013041A1 publication Critical patent/WO1999013041A1/fr
Anticipated expiration legal-status Critical
Priority to US09/619,367 priority patent/US6462003B1/en
Ceased legal-status Critical Current

Links

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
    • C11D13/00—Making of soap or soap solutions in general; Apparatus therefor
    • 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0095—Solid transparent soaps or detergents
    • 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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/002—Non alkali-metal soaps
    • 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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/02—Compositions of detergents based essentially on soap on alkali or ammonium soaps

Definitions

  • the present invention relates to a transparent solid stone and a transparent stone dough. More specifically, the invention does not require fine adjustment of the amount of water or an aging period until the weight is reduced.
  • the present invention relates to a transparent solid stone and a transparent stone or dough that can be easily produced and have good transparency and stability over time in weight.
  • BACKGROUND ART Transparent stones are widely used as detergents because they are aesthetically pleasing and have excellent safety and detergency.
  • transparent stones contain a moisture-absorbing component such as a polysaccharide as an essential component in order to provide transparency, and also contain a volatile component such as ethanol.
  • a volatile component such as ethanol.
  • the transparent solid stone II if the moisture-absorbing component absorbs moisture, the transparency is rather reduced.
  • the transparency of the transparent stone portion will be increased by the moisture contained in the opaque stone.
  • the stripes were lost and the stripes became unclear.
  • some of the transparent solid stones actually used contain sorbitol, which is a polysaccharide, in order to increase the transparency. Turbidity, and the temporal stability of the transparency is not impaired. Therefore, there has been a demand for a transparent stone which can be easily produced without requiring fine adjustment of the amount of water and aging period, and which has excellent transparency and stability over time of weight.
  • the present inventors have conducted intensive studies on transparent solid stones and transparent stones which are easy to produce and have good stability. As a result, the inventors have determined that they can be used for saponification. By using sodium hydroxide and organic amine at a ratio of and the amount of alkali to fatty acid at a predetermined saponification equivalent, a transparent stone can be obtained without using polysaccharides, alcohols and the like as essential components. Further, they found that this transparent stone was easy to produce and had good stability, and completed the present invention.
  • the present invention relates to a stone mainly composed of a salt of a fatty acid, which is obtained by saponifying a fatty acid or animal or vegetable oil and an alkali,
  • Triethanolamine is particularly preferred as the organic amine.
  • the present invention relates to a stone dough mainly comprising a salt of a fatty acid, which is obtained by saponifying a fatty acid or animal or vegetable oil and an alkali, 1)
  • the alkali force is sodium hydroxide and an organic amine, wherein the molar ratio of sodium hydroxide to organic amine is 1: 0.8 to 1: 2,
  • the transparent stone dough of the present invention can be solidified as pellets.
  • the present invention also relates to a transparent solid stone obtained by molding the transparent stone.
  • transparent means a state that is substantially transparent and has little turbidity, and means that the transmittance of visible light is approximately 25% or more. Also,
  • Transparent is not limited to colorless and transparent ones.
  • Transparent solid stone ⁇ is a concept used for a solid formed and solidified in a use form, The state before being molded into ⁇ is referred to as “transparent stone ⁇ cloth”. Further, in the present invention, the “transparent solid stone” includes a stone which is partly transparent in a usage form.
  • spontaneousification equivalent refers to the minimum amount of alcohol required to convert all fatty acids or animal and vegetable oils into salts of fatty acids, that is, stones.
  • the transparent solid stone and the transparent stone dough of the present invention are transparent stones that do not contain polysaccharides or alcohols such as sorbitol and ethanol as essential components. Therefore, unlike transparent stones containing polysaccharides, turbidity due to moisture absorption, crystal precipitation, and the like are not easily generated, and the transparency with time is excellent. Further, since the transparent solid stones and the transparent stones of the present invention do not require moisture-absorbing components such as polysaccharides, the labor for adjusting the water content is reduced, and the volatile components such as alcohol reach equilibrium and the weight is reduced. The production is easy because it is not essential to wait for the aging period until the temperature stops.
  • the transparent solid stone ⁇ of the present invention is obtained by saponifying a fatty acid or an animal or vegetable oil and an alcohol.
  • stones mainly composed of salts of fatty acids are mainly composed of
  • the alcohol is sodium hydroxide and organic amine, and the molar ratio of sodium hydroxide to organic amine is 1: 0.8 to 1: 2;
  • the amount of the alkali is 2 to 3 saponification equivalents to a fatty acid or animal or vegetable oil.
  • organic amine examples include diethanolamine, triethanolamine, triethylamine, trimethylamine, and getylamine. Among them, triethanolamine is particularly preferable.
  • One organic amine may be used alone, or two or more organic amines may be used in combination.
  • the amount of alcohol in the saponification of fatty acids or animal and vegetable oils and oils is preferably 2 to 3 saponification equivalents to the fatty acids or animal and vegetable oils, more preferably 2.1 to 2. 9 saponification equivalent, more preferably 2.2 to 2.7 saponification equivalent o
  • the term "saponification equivalent” as used in the present invention refers to the minimum amount of alkali required to convert all fatty acids or animal and vegetable oils into salts of fatty acids, i.e., stone, and the amount is defined as 1 saponification equivalent.
  • the amount of alkali that is equivalent to 1 saponification can be determined, for example, by calculating the amount of an acid derived from a fatty acid from the weight and the molecular weight of the fatty acid, and calculating the amount of alkali required for neutralizing the acid.
  • the ratio of sodium hydroxide to the organic amine is preferably 1: 0.8 to 1: 2 by molar ratio, more preferably 1: 0.9 to 1: 1.9, and further preferably, 1: 1-1: 1.8.
  • the fatty acid or animal or vegetable oil used in the transparent solid stone of the present invention may be any one which is generally used as a base of stone.
  • Specific examples of the fatty acid include stearic acid, lauric acid, myristic acid, palmitic acid, behenic acid and the like, and may be a synthesized one or a naturally occurring one.
  • Specific examples of animal and vegetable oils include beef tallow, coconut oil, hydrogenated coconut oil, and the like. Fatty acids that have been hydrolyzed in advance and used may be used, or may be used as they are.
  • the amount of the fatty acid charged as a raw material to the transparent solid stone of the present invention is preferably 30 to 60% by weight, more preferably 35 to 57% by weight. %, And more preferably 37 to 55% by weight.
  • the amount of triethanolamine to be charged is preferably 30 to 50% by weight, more preferably 31 to 47% by weight, and still more preferably 32 to 45% by weight.
  • the amount of sodium hydroxide charged is preferably 5 to 10% by weight, more preferably 5.5 to 9.5% by weight, and even more preferably 6 to 9% by weight.
  • optional components generally used in stones can be blended in addition to the above essential components as long as the effects of the present invention are not impaired.
  • Such optional components include, for example, antioxidants such as BHT, chelating agents such as EDTA and hydroxyethanediphosphonic acid, preservatives such as methylparaben, pigments, pigments, powders, iris foil and titanium Pearl agents such as My power, fragrances, surfactants such as POE-added sodium alkyl sulfate, monohydric or polyhydric alcohols or polysaccharides such as ethanol, glycerin, sucrose, maltitol, sorbitol, and honey .
  • the transparency may be impaired to some extent depending on the amount added. Despite the fact, it can be a stone with a bright shine.
  • the transparent solid stone ⁇ of the present invention can be produced according to a normal method for producing a transparent solid stone ⁇ .
  • it can be manufactured by a frame kneading method in which a mixture of a fatty acid or animal or vegetable oil and an alkali is saponified, and if necessary, a mixture of other components is heated and melted, poured into a mold, and cooled and solidified.
  • the transparent stone dough of the present invention is obtained by saponifying a fatty acid or animal or vegetable oil and an alkali, and is mainly made of a salt of a fatty acid.
  • the amount of the alkali is 2 to 3 saponification equivalents to a fatty acid or animal or vegetable oil.
  • the organic amine specifically, diethanolamine, triethanolamine, triethylamine, trimethylamine, getylamine and the like are exemplified as preferable ones, and among these, triethanolamine is particularly preferable.
  • One organic amine may be used alone, or two or more organic amines may be used in combination.
  • the amount of saponified fatty acid or animal or vegetable oil in saponification is preferably 2 to 3 saponification equivalents to the fatty acid or animal or vegetable oil, more preferably 2.1 to 2.9. It is a saponification equivalent, and more preferably, 2.2 to 2.7 saponification equivalent.
  • the molar ratio of sodium hydroxide to organic amine is 1: 0.8 to 1: 2, preferably, more preferably, 1: 0.9 to 1: 1.9, and still more preferably. The ratio is 1: 1 to 1: 1.8.
  • the fatty acid or animal or vegetable oil used in the transparent stone dough of the present invention may be any one that is generally used as a base of stone.
  • Specific examples of the fatty acid include stearic acid, lauric acid, myristic acid, palmitic acid, behenic acid and the like, and may be a synthesized one or a naturally occurring one.
  • Specific examples of animal and vegetable oils include beef tallow, coconut oil, hydrogenated coconut oil, and the like. Those that have been hydrolyzed in advance to form fatty acids may be used, or may be used as they are.
  • the amount of fatty acid charged as a raw material to the transparent stone dough of the present invention is preferably 30 to 60% by weight, more preferably 35 to 57% by weight, More preferably, it is 37 to 55% by weight.
  • the amount of triethanolamine to be charged is preferably 30 to 50% by weight, more preferably 31 to 47% by weight, and still more preferably 32 to 45% by weight.
  • the amount of sodium hydroxide to be charged is preferably 5 to 10% by weight, more preferably 5.5 to 9.5% by weight, and still more preferably 6 to 9% by weight.
  • optional components generally used in stone can be added in addition to the above essential components.
  • optional components include, for example, antioxidants such as BHT, chelating agents such as EDTA and hydroxyethanediphosphonic acid, preservatives such as methylparaben, pigments, pigments, powders, iris foil and titanium Pearl agents such as my power, fragrances, surfactants such as POE-added sodium alkyl sulfate, ethanol, glycerin, sucrose, Monohydric or polyhydric alcohols or polysaccharides such as maltitol, sorbitol and honey are mentioned.
  • the transparency may be impaired to some extent depending on the amount added. Despite the fact, it can be a stone with a bright shine.
  • the transparent stone dough of the present invention can be manufactured according to a usual stone dough manufacturing method.
  • the transparent stone dough of the present invention saponifies a fatty acid or the like with an alkali, and if necessary, adds other components, kneads these components, rolls, extrudes and solidifies the stone. ⁇ Can be made into dough, that is, pellets.
  • the pellets can be subjected to processing such as pressure molding, that is, a transparent solid stone can be obtained by a mechanical kneading method.
  • a transparent solid stone having a striped pattern can be formed by press-molding the transparent stone material of the present invention into a pellet and a pellet made from ordinary opaque stone material. can get.
  • a molded object such as a flower is made of opaque stone, and the molded object is embedded in the transparent stone of the present invention by the frame kneading method and molded, whereby the transparent solid stone in which the molded object is embedded is obtained. ⁇ can be obtained.
  • Example 1 Example 2
  • Example 3 Palm oil fatty acid 4 0 4 0 4 0 Tallow fatty acid 1 6 0 1 6 0 1 6 0
  • Sodium hydroxide 3 4 2 9 26
  • Water 8 6 8 1 7 9 Properties of pellet Transparent solid Transparent solid Water content of transparent solid pellet (% by weight) 5.4.6.24.8 Component separation
  • Example 4 Example 5
  • Example 6 Coconut oil Fatty acid 4 0 4 0 4 0 Tallow fatty acid 1 6 0 1 6 0 1 6 0
  • Water 8 6 7 9 8 4 Pellet Properties Transparent solid Transparent solid Transparent solid Water content of pellets (% by weight) 6.15.5.5.6 Table 2 (Unit: wt%) Ingredients Example 1 Example 2
  • Example 3 Coconut oil fatty acid 10.2 1 0.0 9.7 Tallow fatty acid 40.9 40.
  • Examples 7 to 12 The pellet-shaped transparent stones and doughs of Examples 1 to 6 were molded under pressure to obtain transparent solid stones. Even if this transparent solid stone was stored at 40 for one month, the weight change was less than 5%, the transparency was not changed, and no crystals were precipitated.
  • Example 13 According to the weighed-in prescription shown in Table 4 below, transparent stone dough was produced. Specifically, the ingredients shown in Table 4 were weighed into a heated kneader, kneaded at 80 with kneading for 2 hours, and pelletized with a hot roll and a pelletizer to obtain transparent stone and dough as pellets. Was. According to the formula in Table 4, the amount of alkali relative to the fatty acid is determined by 2.45 saponification equivalent.
  • Example 14 The transparent solid material of Example 13 was molded under pressure to obtain a transparent solid stone. Even when this transparent solid stone was stored at 40 for one month, there was no precipitation of crystals and no change in transparency.
  • Example 15 A transparent stone dough was produced according to the weighed-in prescription in Table 5 below. Specifically, the ingredients listed in Table 5 were weighed into a heating pan, kneaded at 80 for 2 hours, and pelletized with a hot roll and pelletizer. I got it. According to the formulation in Table 5, the amount of alkali relative to fatty acid is determined by 2.45 saponification equivalents.
  • Example 16 A transparent solid stone was obtained by press-molding the transparent stone material of Example 15 to obtain a transparent solid stone. This transparent solid stone did not change its weight even when stored at 40 ° C for one month. Was.
  • Example 17 According to the weighing-in prescription of Table 6, stone fabric was prepared. Specifically, the ingredients in Table 6 were weighed into a heating canister, kneaded at 80 ° C for 2 hours, and pelletized with a hot roll and a pelletizer. Obtained. According to the formulation in Table 6, the amount of alkali relative to fatty acid is 2.45 saponification equivalents.
  • Example 18 According to the weighing-in prescription of Table 7, transparent stone dough was produced. More specifically, the ingredients in Table 6 were weighed into a heating bottle, kneaded at 80 ° C. for 2 hours, and pelletized by a hot roll and a pelletizer. ⁇ The dough was obtained as a pellet. According to the formulation in Table 7, the amount of alkali relative to fatty acid is 2.45 saponification equivalents.
  • Example 19 The pellets of Example 17 were heated and melted, poured into a silicone rubber mold, and solidified to produce a rose shaped article. This was placed in a frame, quietly transparent stones ⁇ locations Example 1 8 were heated and dissolved pouring, cooling and solidifying are allowed to c the transparent solid stone ⁇ to obtain a flower containing transparent bar stone ⁇ is 4 0, There was no change in the transparency of the transparent part after storage for one month, and there was no change in weight.
  • the transparent solid stone I and the transparent stone I dough of the present invention can be easily produced without the need for fine adjustment of the water content and aging period until the weight is reduced, and the transparency is high. Also, the stability with time of weight is good.

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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)

Abstract

L'invention concerne un savon solide transparent ou une pâte de savon transparente se composant principalement d'un sel d'acide gras préparé par saponification d'un acide gras, ou d'une huile animale ou végétale avec un alcali, 1) l'alcali comprenant de l'hydroxyde de sodium et une amine organique telle que la triéthanolamine, le rapport molaire entre l'hydroxyde de sodium et l'amine organique étant compris entre (1:0,8) et (1:2); et 2) la quantité d'alcali étant de 2 à 3 équivalents de saponification relativement à la qualité d'acide gras ou d'huile animale ou végétale. Le savon et la pâte de savon peuvent être facilement préparés sans qu'il soit nécessaire de surveiller de près la teneur en eau et la période de vieillissement jusqu'à ce que la réduction du poids cesse, et la stabilité de la transparence et le poids après écoulement de la période précitée sont satisfaisants.
PCT/JP1997/003137 1996-05-22 1997-09-05 Savon solide transparent et pate de savon transparente Ceased WO1999013041A1 (fr)

Priority Applications (10)

Application Number Priority Date Filing Date Title
JP12728396A JP3378725B2 (ja) 1996-05-22 1996-05-22 透明固形石鹸及び透明石鹸生地
PCT/JP1997/003137 WO1999013041A1 (fr) 1996-05-22 1997-09-05 Savon solide transparent et pate de savon transparente
CA002270381A CA2270381A1 (fr) 1997-09-05 1997-09-05 Savon solide transparent et pate de savon transparente
EP97939200A EP0947579B1 (fr) 1997-09-05 1997-09-05 Procede de fabrication de savon solide transparent ou pate de savon transparente
AU41358/97A AU720810B2 (en) 1997-09-05 1997-09-05 Transparent solid soap and transparent soap material
BR9712732-9A BR9712732A (pt) 1997-09-05 1997-09-05 Sabão sólido transparente, e, material de sabão transparente.
US09/297,593 US6156714A (en) 1996-05-22 1997-09-05 Transparent solid soap and transparent soap stock comprising sodium hydroxide and organic amine
NZ335346A NZ335346A (en) 1997-09-05 1997-09-05 Transparent solid soap and transparent soap material; obtained by saponifying fatty acid or animal/vegetable oil with sodium hydroxide and an organic amine
DE69736071T DE69736071T2 (de) 1997-09-05 1997-09-05 Verfahren zur herstellung von transparenten festen seifen sowie von transparentem seifenvorrat
US09/619,367 US6462003B1 (en) 1997-09-05 2000-07-19 Transparent solid soap and transparent soap material

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP12728396A JP3378725B2 (ja) 1996-05-22 1996-05-22 透明固形石鹸及び透明石鹸生地
PCT/JP1997/003137 WO1999013041A1 (fr) 1996-05-22 1997-09-05 Savon solide transparent et pate de savon transparente

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US09/619,367 Continuation US6462003B1 (en) 1997-09-05 2000-07-19 Transparent solid soap and transparent soap material

Publications (1)

Publication Number Publication Date
WO1999013041A1 true WO1999013041A1 (fr) 1999-03-18

Family

ID=14181076

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP1997/003137 Ceased WO1999013041A1 (fr) 1996-05-22 1997-09-05 Savon solide transparent et pate de savon transparente

Country Status (5)

Country Link
EP (1) EP0947579B1 (fr)
AU (1) AU720810B2 (fr)
CA (1) CA2270381A1 (fr)
DE (1) DE69736071T2 (fr)
WO (1) WO1999013041A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60188500A (ja) * 1984-03-08 1985-09-25 三和化学工業株式会社 成型透明石鹸の製造方法
JPS63275700A (ja) * 1987-04-30 1988-11-14 ニュウトロゼナ　コーポレイション 透明石鹸とその連続製造法
JPH01292097A (ja) * 1988-03-31 1989-11-24 Unilever Nv 透明棒型石けん
JPH04213398A (ja) * 1990-06-21 1992-08-04 Kanebo Ltd 透明石鹸組成物

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1847437A (en) * 1929-10-24 1932-03-01 Moscowitz Abraham Detergent
US4297230A (en) * 1979-02-06 1981-10-27 The Procter & Gamble Company Non-crystallizing transparent soap bars
ZA882340B (en) * 1988-03-31 1989-12-27 Unilever Plc Transparent soap bar
US5728663A (en) * 1996-07-02 1998-03-17 Johnson & Johnson Consumer Products, Inc. Clear, colorless soap bar with superior mildness, lathering and discolorization resistence

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60188500A (ja) * 1984-03-08 1985-09-25 三和化学工業株式会社 成型透明石鹸の製造方法
JPS63275700A (ja) * 1987-04-30 1988-11-14 ニュウトロゼナ　コーポレイション 透明石鹸とその連続製造法
JPH01292097A (ja) * 1988-03-31 1989-11-24 Unilever Nv 透明棒型石けん
JPH04213398A (ja) * 1990-06-21 1992-08-04 Kanebo Ltd 透明石鹸組成物

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP0947579A4 *

Also Published As

Publication number Publication date
CA2270381A1 (fr) 1999-03-18
AU4135897A (en) 1999-03-29
AU720810B2 (en) 2000-06-15
DE69736071D1 (de) 2006-07-20
EP0947579A1 (fr) 1999-10-06
DE69736071T2 (de) 2006-12-21
EP0947579A4 (fr) 2001-03-28
EP0947579B1 (fr) 2006-06-07

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