EP0506751B1 - Utilisation d'une combinaison de tensio-actifs non ioniques - Google Patents
Utilisation d'une combinaison de tensio-actifs non ioniques Download PDFInfo
- Publication number
- EP0506751B1 EP0506751B1 EP91901279A EP91901279A EP0506751B1 EP 0506751 B1 EP0506751 B1 EP 0506751B1 EP 91901279 A EP91901279 A EP 91901279A EP 91901279 A EP91901279 A EP 91901279A EP 0506751 B1 EP0506751 B1 EP 0506751B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- carbon atoms
- alkyl radical
- general formula
- linear
- radical containing
- 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
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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/825—Mixtures of compounds all of which are non-ionic
- C11D1/8255—Mixtures of compounds all of which are non-ionic containing a combination of compounds differently alcoxylised or with differently alkylated chains
-
- 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
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
-
- 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
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
- C11D1/721—End blocked ethers
-
- 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
- C11D1/66—Non-ionic compounds
- C11D1/722—Ethers of polyoxyalkylene glycols having mixed oxyalkylene groups; Polyalkoxylated fatty alcohols or polyalkoxylated alkylaryl alcohols with mixed oxyalkylele groups
Definitions
- the present invention relates to the use of a combination of nonionic surfactants - optionally with conventional additives - for cleaning hard surfaces in the spraying process. So-called “industrial cleaners” are usually used for such tasks.
- Industrial cleaners of this type are mainly used in the automotive industry and their supplier industries for cleaning and passivation, primarily in spray cleaning systems. They are suitable for intermediate and final cleaning without cutting as well as machined parts in unit and assembly plants. Practically all relevant materials, such as iron and steel, aluminum, silumen, copper, brass, zinc and plastics, can be treated and the majority of all contaminations on an organic or inorganic basis, such as cooling lubricants, rust protection oils, processing oils, drawing aids, pigments and light metal abrasion, can be removed. Such cleaning agents can also be used in customary immersion processes, but their use in the spraying process is usually preferred.
- cleaning agents of this type generally contain substances which are capable of an undesirable one Counteract foam development.
- foam-inhibiting additives is in most cases due to the fact that the contaminants detached from the substrates and accumulating in the cleaning baths act as foaming agents.
- anti-foaming agents may also be necessary due to the fact that the cleaning agents themselves contain constituents which give rise to undesirable foaming under the given working conditions - ie in particular in the case of spraying processes, for example anionic surfactants or nonionic surfactants foaming at the respective working temperature.
- Such formulations can be used both for cleaning hard surfaces and for washing textiles.
- Such surfactant mixtures are used in aqueous cleaning agents for cleaning hard surfaces, in particular also for spray cleaning at temperatures below 50 ° C.
- the object of the present invention was to provide surfactant combinations for cleaning hard surfaces which have low-foaming properties in the entire temperature range relevant to the application, namely in the range from 15 to 80 ° C., and are therefore suitable for use in the spraying process.
- these surfactant combinations should have a high cleaning ability and excellent wetting properties compared to the substrates treated with them; further should these surfactant combinations can be easily assembled with additives common in industrial cleaners, allow the cleaning agent solutions to run off the treated substrate surfaces without stains and have demulsifying properties with regard to non-self-emulsifying oils and fats.
- R 1 represents a linear or branched alkyl radical or alkenyl radical having 6 to 18 carbon atoms.
- the following radicals are therefore suitable as substituent R 1: n-hexyl, n-heptyl, n-octyl, n-nonyl, n-decyl, n-undecyl, n-dodecyl, n-tridecyl, n-tetradecyl, n-pentadecyl , n-hexadecyl, n-heptadecyl and n-octadecyl and the branched chain isomers of the alkyl radicals mentioned.
- R 1 can also mean the unsaturated alkyl radicals (alkenyl radicals) with a number of carbon atoms in the above range, which can likewise be linear or branched.
- component a those compounds of the general formula (I) in which R 1 is a linear alkyl radical or alkenyl radical having 6 to 18 carbon atoms.
- R 1 is a linear alkyl radical or alkenyl radical having 6 to 18 carbon atoms.
- R 2 represents a linear or branched alkyl radical or alkenyl radical with 6 to 18 carbon atoms or a cyclic alkyl radical with 5 to 6 carbon atoms. Suitable substituents R 2 are therefore all those radicals which have already been explained above in connection with the substituent R 1 of the general formula (I).
- the number of ethoxy radicals in the molecule - index p - is in the range from 2 to 10.
- the substituent A in the general formula (II) stands for propoxy radicals, the number of propoxy radicals - index (q + r) - in the range from 2 to 8 lies.
- components b of the general formula (II) are preferably used as component b in which R 2 is a linear alkyl radical having 8 to 18 carbon atoms, p is a number in the range from 2 to 5 and A is propoxy radicals, and the sum (q + r) is a number in the range 4 to 6.
- the reaction product of technical lauryl alcohol - which has alkyl radicals with 12 to 18 carbon atoms (thereof about 80% with 12 to 14 carbon atoms) - with 2 to 4 is used as the surfactant component b Moles of ethylene oxide and 4 to 6 moles of propylene oxide or the reaction product of n-octanol with 2 to 6 moles of ethylene oxide and 2 to 5 moles of propylene oxide.
- the surfactant combinations to be used according to the invention contain, as additional component c, at least one alk (en) yl ethoxylate mixed ether of the general formula (III) R3-O- (CH2CH2O) s -R4 (III) in which R3 is a linear or branched alkyl radical or alkenyl radical with 6 to 18 carbon atoms or a cyclic alkyl radical with 5 to 6 carbon atoms, s is a number in the range from 2 to 12 and R4 is a linear or branched alkyl radical with 1 to 8 carbon atoms -Atoms mean, the weight ratio of components (a + b): c being in the range from 1: (0.1 to 4).
- R3 therefore stands for a linear or branched alkyl radical or alkenyl radical with 6 to 18 carbon atoms or a cyclic alkyl radical with 5 to 6 carbon atoms.
- Suitable substituents R3 are therefore all those radicals which have already been explained above in connection with the substituent R1 of the general formula (I).
- the number of ethoxy radicals in the molecule - index s - is here in the range from 2 to 12.
- the substituent R4 in the general formula (III) stands for a linear or branched alkyl radical with 1 to 8 C atoms; thus for methyl, ethyl, n-propyl, n-butyl, n-pentyl, n-hexyl, n-heptyl, n-octyl and for the corresponding branched-chain isomers.
- alk (en) yl ethoxylate mixed ethers which are also referred to as end group-capped fatty alcohol polyethylene glycol ethers are described in more detail in DE-A-33 15 951, 37 27 378 and 38 00 490.
- the production of these nonionic surfactants is also disclosed in detail in these German published publications.
- At least one alkyl ethoxylate mixed ether of the general formula (III) as additional component c of the surfactant combination, where R 3 is a linear alkyl radical having 8 to 10 carbon atoms, s is a number in the range from 3 to 5 and R4 represent an n-butyl radical.
- Particularly preferred mixed alkyl ethoxylate ethers of the general formula (III) are addition products of 3.5 to 4.5 mol of ethylene oxide onto fatty alcohols having 8 to 10 carbon atoms and etherified with an n-butyl radical.
- the surfactant combinations to be used according to the invention are further characterized by a certain weight ratio of components a: b, which is generally in the range from 10: 1 to 1:10. If only these two components are used in the manner according to the invention, the preferred weight ratio of components a: b is in the range from 2: 1 to 1: 2. However, if the surfactant combination to be used according to the invention contains the additional component c, the weight ratio is of components (a + b): c in the range from 1: 0.1 to 1: 4, preferably in the range from 1: 0.1 to 1: 1.5.
- the surfactant combinations to be used according to the invention are notable for high cleaning power at temperatures in the range from 15 to 80 ° C. They are in the temperature range mentioned can also be used without any problems in the spraying process since they do not cause any undesirable foam development. Further advantages are: very good wetting properties, very good demulsifying properties with regard to non-self-emulsifying oils and fats as well as easy assembly with additives commonly used in industrial cleaners.
- additives which are preferably used in addition to the surfactant combinations to be used according to the invention are: builder substances and / or complexing agents, corrosion inhibitors and bases or acids.
- stabilizers, solubilizers or antimicrobial agents can also be used as additives.
- alkali metal orthophosphates for example, alkali metal orthophosphates, polyphosphates, silicates, borates, carbonates, polyacrylates and gluconates can be used, as well as phosphonic acids or phosphonoalkane carboxylic acids or their water-soluble alkali metal salts, for example 1-hydroxyethane-1,1-diphosphate or 2-phosphonobutane-1,2,4-tricarboxylic acid.
- Straight-chain or branched aliphatic carboxylic acids or their salts are suitable as effective corrosion inhibitors.
- alkanolamine salts of straight-chain or branched monocarboxylic acids with 8 to 11 carbon atoms are used as corrosion inhibitors.
- the aqueous solutions of the surfactant combinations to be used according to the invention can be acidic or also alkaline; accordingly, they contain excess acid or bases, for example sodium hydroxide and / or potassium hydroxide.
- the surfactant combinations to be used according to the invention are produced by simply mixing the individual components.
- Corresponding powdery or liquid cleaning agents are also produced in the same way by mixing the surfactant combinations to be used according to the invention with the other additives and, if appropriate, water.
- cleaning agents of this type contain 1 to 70% by weight, preferably 2 to 20% by weight, of the surfactant combinations to be used according to the invention.
- the surfactant combinations to be used according to the invention are preferably used in the form of application solutions diluted with water.
- Such application solutions preferably contain the surfactant combinations to be used according to the invention in concentrations of 0.0001 to 1.5% by weight, in particular 0.0005 to 0.5% by weight.
- Ready-to-use solutions of this type which are used in the sense of the invention for cleaning hard surfaces in the spray process, can likewise be strongly acidic to strongly alkaline (pH values in the range from 1 to 14) and preferably have pH values in the range from 3.5 to 11 on.
- Such application solutions are prepared by simply mixing the surfactant combinations with water.
- Base Indication of the number of the detergent base used in the respective example according to example 2.
- Proportion means the respective concentration of the surfactant combination based on the detergent base in% by weight.
- component a of the surfactant combination to be used according to the invention - octanol + 4 EO - was tested alone in a test according to Example 3.
- This surfactant was used here in a concentration of 1% by weight in the detergent bases given in Table 1 at spray temperatures between 20 and 70 ° C and a spray pressure of 3 bar - water quality: VEW.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Detergent Compositions (AREA)
- Cosmetics (AREA)
- External Artificial Organs (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Dental Preparations (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Claims (6)
- Utilisation d'une combinaison d'agents tensio-actifs non ioniques à base d'éthoxylates d'alcoyle ou d'alcényle et de éthoxylates/propoxylates d'alcoyle ou d'alcényle en vue du nettoyage de surfaces dures dans un procédé par pulvérisation, caractérisée en ce qu'elle contient les composants suivants :a) au moins un alcoyle ou alcényle éthoxylate de formule générale (I)
R¹-O-(CH₂CH₂O)n -H (I)
dans laquelle R₁ signifie un radical alcoyle linéaire ou ramifié ou un radical alcényle, ayant de 6 à 18 atomes de carbone et n signifie un nombre dans la zone de 2 à 4.
ou dans laquelle R¹ signifie un radical alcoyle linéaire ayant 6 atomes de carbone et n le nombre 6 etb) au moins un alcoyle ou alcényle éthoxypropoxylate de formule générale (II)
R²-O-(CH₂CH₂O)p-A-H (II)
dans laquelle R² signifie un radical alcoyle linéaire ou ramifié ou un radical alcényle ayant de 6 à 18 atomes de carbone ou un radical alcoyle cyclique ayant 5 ou 6 atomes de carbone p est un nombre dans la zone de 2 à 10 et A est un radical du type
-(CH₂-CH(CH₃)-O)q-
et
(CH(CH₃)-CH₂-O)r
pour lequel la somme (q+r) est un nombre dans la zone allant de 2 à 8,
combinaison dans laquelle le rapport pondéral des composants a : b se situe dans la zone de 10 : 1 à 1 : 10. - Utilisation selon la revendication 1, caractérisée en ce que comme composant b de la combinaison d'agents tensio-actifs, on met en oeuvre au moins un alcoyl éthoxylate/propoxylate de formule générale (II), dans laquelle R² est un radical alcoyle linéaire ayant de 8 à 18 atomes de carbone, p est un nombre dans la zone allant de 2 à 5 et A représente les radicaux mentionnés précédemment, formule dans laquelle la somme (q+r) et un nombre dans la zone de 4 à 6.
- Utilisation selon l'une des revendications 1 et 2, caractérisée en ce que la combinaison d'agents tensio-actifs contient comme composant additionnel c au moins un éther mixte d'alcoyle ou d'alcényle d'éthoxylate de formule générale (III)
R³-O-(CH₂CH₂O)s-R⁴ (III)
dans laquelle R³ signifie un radical alcoyle linéaire ou ramifié ou un radical alcényle ayant de 6 à 18 atomes de carbone ou un radical alcoyle cyclique ayant de 5 à 6 atomes de carbone, s signifie un nombre dans la zone de 2 à 12 et R⁴ signifie un radical alcoyle linéaire ou ramifié ayant de 1 à 8 atomes de carbone, combinaison
dans laquelle le rapport pondéral des composants (a+b) : c se situe dans la zone de 1 : (0,1 à 4). - Utilisation selon la revendication 3, caractérisée en ce que comme composant supplémentaire c) de la combinaison d'agents tensio-actifs, on met en oeuvre au moins un éther mixte d'alcoyle d'éthoxylate de formule générale (III) dans laquelle R³ signifie un radical alcoyle linéaire ayant de 8 à 10 atomes de carbone, s signifie un nombre dans la zone allant de 3 à 5 et R⁴ signifie un radical n-butyle.
- Utilisation selon l'une des revendications 1 à 4, caractérisée en ce que la combinaison d'agents tensio-actifs contient en plus des substances de structuration, et/ou des agents complexants, des inhibiteurs de corrosion ainsi que des bases ou des acides.
- Utilisation selon l'une des revendication 1 à 5, caractérisée en ce que la combinaison d'agents tensio-actifs est mise en oeuvre dans des solutions d'utilisation diluées avec de l'eau à des concentrations allant de 0,0001 à 1,5 % en poids, de préférence de 0,005 à 0,5 % en poids.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3942727 | 1989-12-22 | ||
DE3942727A DE3942727A1 (de) | 1989-12-22 | 1989-12-22 | Verwendung einer kombination nichtionischer tenside |
PCT/EP1990/002170 WO1991009925A2 (fr) | 1989-12-22 | 1990-12-13 | Utilisation d'une combinaison de tensio-actifs non ioniques |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0506751A1 EP0506751A1 (fr) | 1992-10-07 |
EP0506751B1 true EP0506751B1 (fr) | 1994-06-08 |
Family
ID=6396281
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP91901279A Expired - Lifetime EP0506751B1 (fr) | 1989-12-22 | 1990-12-13 | Utilisation d'une combinaison de tensio-actifs non ioniques |
Country Status (12)
Country | Link |
---|---|
EP (1) | EP0506751B1 (fr) |
JP (1) | JPH05502259A (fr) |
AT (1) | ATE106937T1 (fr) |
BR (1) | BR9007941A (fr) |
CA (1) | CA2072009A1 (fr) |
DE (2) | DE3942727A1 (fr) |
DK (1) | DK0506751T3 (fr) |
ES (1) | ES2055582T3 (fr) |
PT (1) | PT96342A (fr) |
TR (1) | TR25486A (fr) |
WO (1) | WO1991009925A2 (fr) |
ZA (1) | ZA9010356B (fr) |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0606325B1 (fr) * | 1991-09-26 | 1995-11-29 | BOUS, Klaus | Liquide de nettoyage, en particulier pour trousses de secours, et son utilisation |
DE4237178A1 (de) * | 1992-11-04 | 1994-05-05 | Henkel Kgaa | Wäßriges Tensidkonzentrat |
US5759979A (en) * | 1993-04-05 | 1998-06-02 | Henkel Kommanditgesellschaft Auf Aktien | Detergent mixtures comprising APG and fatty alcohol polyglycol ether |
DE4426889A1 (de) * | 1994-07-29 | 1996-02-01 | Hoechst Ag | Mischungen von Alkoxylaten als schaumdämpfendes Mittel und deren Verwendung |
US5612305A (en) * | 1995-01-12 | 1997-03-18 | Huntsman Petrochemical Corporation | Mixed surfactant systems for low foam applications |
ATE493374T1 (de) * | 2002-04-26 | 2011-01-15 | Basf Se | Alkoxylatgemische und diese enthaltende waschmittel |
DE10313461A1 (de) * | 2003-03-26 | 2004-10-07 | Henkel Kgaa | Reinigungslösung und Reinigungsverfahren für Lackleitungen und/oder Lackauftragsgeräte |
DE102005037971A1 (de) * | 2005-08-11 | 2007-02-15 | Clariant Produkte (Deutschland) Gmbh | Zusammensetzungen enthaltend Fettalkoholalkoxylate |
CN101578130A (zh) | 2007-01-11 | 2009-11-11 | 陶氏环球技术公司 | 烷氧基化物混合物表面活性剂 |
DE102007019457A1 (de) * | 2007-04-25 | 2008-10-30 | Basf Se | Maschinengeschirrspülmittel mit ausgezeichneter Klarspülleistung |
DE102007019458A1 (de) * | 2007-04-25 | 2008-10-30 | Basf Se | Phosphatfreies Maschinengeschirrspülmittel mit ausgezeichneter Klarspülleistung |
JP2014141668A (ja) * | 2012-12-27 | 2014-08-07 | Sanyo Chem Ind Ltd | 電子材料用洗浄剤 |
AU2017267050B2 (en) | 2016-05-17 | 2020-03-05 | Unilever Global Ip Limited | Liquid laundry detergent compositions |
EP3933020B1 (fr) * | 2019-02-26 | 2023-09-27 | Nippon Kayaku Kabushiki Kaisha | Utilisation d'une solution de nettoyage et procédé de nettoyage d'imprimante jet d'encre |
CN113754371B (zh) * | 2021-08-30 | 2022-10-21 | 广东盛瑞科技股份有限公司 | 高石粉含量的泡沫轻质土及其制备方法 |
WO2023178580A1 (fr) * | 2022-03-24 | 2023-09-28 | Ecolab Usa Inc. | Émulsifiant pour la lessive comprenant un tensioactif et un solvant |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3707506A (en) * | 1968-08-19 | 1972-12-26 | Basf Wyandotte Corp | Nonionic detergent compositions for cleaning polyester fabrics |
ATE68519T1 (de) * | 1986-07-24 | 1991-11-15 | Henkel Kgaa | Schaumarme und/oder schaumdaempfende tensidgemische und ihre verwendung. |
DE3643895A1 (de) * | 1986-12-22 | 1988-06-30 | Henkel Kgaa | Fluessige nichtionische tensidmischungen |
FR2614898B1 (fr) * | 1987-05-06 | 1994-01-07 | Sandoz Sa | Compositions detergentes liquides biodegradables |
DE3818014A1 (de) * | 1988-05-27 | 1989-11-30 | Henkel Kgaa | Schaumdrueckende alkylpolyglykolether fuer reinigungsmittel (ii) |
DE3818062A1 (de) * | 1988-05-27 | 1989-12-07 | Henkel Kgaa | Schaumdrueckende alkylpolyglykolether fuer reinigungsmittel (i) |
-
1989
- 1989-12-22 DE DE3942727A patent/DE3942727A1/de not_active Withdrawn
-
1990
- 1990-12-06 TR TR90/1164A patent/TR25486A/xx unknown
- 1990-12-13 EP EP91901279A patent/EP0506751B1/fr not_active Expired - Lifetime
- 1990-12-13 AT AT91901279T patent/ATE106937T1/de not_active IP Right Cessation
- 1990-12-13 JP JP3501672A patent/JPH05502259A/ja active Pending
- 1990-12-13 DK DK91901279.9T patent/DK0506751T3/da active
- 1990-12-13 CA CA002072009A patent/CA2072009A1/fr not_active Abandoned
- 1990-12-13 WO PCT/EP1990/002170 patent/WO1991009925A2/fr active IP Right Grant
- 1990-12-13 DE DE59006082T patent/DE59006082D1/de not_active Expired - Fee Related
- 1990-12-13 BR BR909007941A patent/BR9007941A/pt unknown
- 1990-12-13 ES ES91901279T patent/ES2055582T3/es not_active Expired - Lifetime
- 1990-12-21 PT PT96342A patent/PT96342A/pt not_active Application Discontinuation
- 1990-12-21 ZA ZA9010356A patent/ZA9010356B/xx unknown
Also Published As
Publication number | Publication date |
---|---|
DE3942727A1 (de) | 1991-06-27 |
JPH05502259A (ja) | 1993-04-22 |
WO1991009925A3 (fr) | 1992-01-09 |
BR9007941A (pt) | 1992-10-06 |
ES2055582T3 (es) | 1994-08-16 |
EP0506751A1 (fr) | 1992-10-07 |
CA2072009A1 (fr) | 1991-06-23 |
ZA9010356B (en) | 1991-08-28 |
TR25486A (tr) | 1993-05-01 |
DE59006082D1 (de) | 1994-07-14 |
ATE106937T1 (de) | 1994-06-15 |
WO1991009925A2 (fr) | 1991-07-11 |
DK0506751T3 (da) | 1994-10-24 |
PT96342A (pt) | 1991-09-30 |
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