EP0084657A1 - Agents de lavage granulaires très moussants séchés par pulvérisation avec une stabilité élevée des granulations et procédé pour sa fabrication - Google Patents

Agents de lavage granulaires très moussants séchés par pulvérisation avec une stabilité élevée des granulations et procédé pour sa fabrication Download PDF

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Publication number
EP0084657A1
EP0084657A1 EP82111827A EP82111827A EP0084657A1 EP 0084657 A1 EP0084657 A1 EP 0084657A1 EP 82111827 A EP82111827 A EP 82111827A EP 82111827 A EP82111827 A EP 82111827A EP 0084657 A1 EP0084657 A1 EP 0084657A1
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EP
European Patent Office
Prior art keywords
weight
sodium
composition according
component
components
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.)
Granted
Application number
EP82111827A
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German (de)
English (en)
Other versions
EP0084657B1 (fr
Inventor
Herbert Dr. Reuter
Wolfgang Dr. Seiter
Ingo Wegener
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Priority to AT82111827T priority Critical patent/ATE18070T1/de
Publication of EP0084657A1 publication Critical patent/EP0084657A1/fr
Application granted granted Critical
Publication of EP0084657B1 publication Critical patent/EP0084657B1/fr
Expired legal-status Critical Current

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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
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0094—High foaming compositions
    • 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/02—Preparation in the form of powder by spray drying
    • 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
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates
    • 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
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites

Definitions

  • the present invention relates to a detergent which has a high content of anionic surfactants and is characterized by a grain structure which is resistant to mechanical or unfavorable weather-related influences and is particularly suitable for washing by hand.
  • Such agents are particularly suitable for use in developing countries, where mostly still under relatively simple conditions, i.e. is washed in the tub and without additional heat.
  • Detergents are already known which consist of compact granules and detergent substances incorporated therein, for example DE-OS 25 36 594 or DE-OS 27 42 683 (US Pat. No. 4,269,722). These are so-called carrier grains, which are produced by spray drying or targeted shaping without the addition of detergents and are subsequently subjected to liquid or melted nonionic surfactants. Such a procedure requires several process steps and is comparatively complex. Such a procedure is out of the question for salt-like anionic surfactants. In addition, such powders have a very compact grain structure and a comparatively high bulk density of over 500 g / l, mostly from 600 to 800 g / 1. Such dense, specifically heavy detergent granules dissolve very slowly in cold or moderately heated water.
  • granular detergents can also be produced by spray drying, but in general, relatively soft, loose powders with a hollow spherical structure are produced when spray-drying conventional detergent compositions. Their bulk density is generally well below 500 g / l and is generally 200 to 350 g / l.
  • Such powders which are usually produced by spraying a water-containing detergent paste under high pressure by means of fixed nozzles, have an optimal solution behavior, but are relatively sensitive to mechanical stress. Older drying systems equipped with rotating spray elements deliver a firmer, but much finer grain with a high dust content. Such powders are very prone to clumping and have an unfavorable pouring behavior.
  • Another problem is the spray drying of detergents with high, ie. H. more than 40% of the organic matter content at the high drying temperatures usually prevailing in the spray towers due to the risk of dust explosions and autoxidation processes which can lead to browning of the powder.
  • Preferred agents are those in which the sum of components (A) and (B) is 40 to 48% by weight and the sum of components (C) to (G) is 52 to 60% by weight.
  • Component (A) consists of linear sodium alkylbenzenesulfonate with 10 to 14 carbon atoms in the alkyl chain.
  • a preferred example of this class of compounds is dodecylbenzenesulfonate.
  • Component (B) is sodium fatty alcohol sulfates, which are derived from saturated and / or monounsaturated primary fatty alcohols of natural or synthetic origin, and preferably 12 to 18
  • Examples include coconut or; Tallow fatty alcohols, oleyl alcohol and synthetic alcohols obtainable by ethylene polymerization or oxosynthesis, the latter consisting of mixtures of linear and ⁇ -methyl-branched alcohols.
  • coconut fatty alcohol sulfates and similarly composed mixtures of saturated C 12 -C 18 fatty alcohol sulfates are particularly preferred.
  • the surfactants contained in the agents can consist exclusively of alkylbenzenesulfonates.
  • a surfactant mixture is preferably used in which the amount of the fatty alcohol sulfates (component B) is such that the content of this component (B) in the detergents is up to 15% by weight, in particular 3-10% by weight.
  • the amount of alkylbenzenesulfonates should be reduced accordingly, so that the total proportion of surfactants does not exceed 50% by weight and the proportion of alkylbenzenesulfonate, in particular 35 to 45% by weight.
  • the proportion of sodium tripolyphosphate (component C), based on anhydrous salt, is 5 to 25% by weight, preferably 8 to 20% by weight and in particular 10 to 17% by weight.
  • the tripolyphosphate is usually present as hexahydrate, wherein the attributable water content of the component (G) is alculated train.
  • Tripolyphosphate in a mixture with small amounts of its hydrolysis products, ie diphosphate and orthophosphate, formed in the aqueous batch or in the course of spray drying, but their proportion is less than 20% by weight, preferably less than 15%, of the tripolyphosphate used for spray drying.
  • Component (D) consists of fine-crystalline sodium aluminum silicates of the formula (I) given above which are capable of cation exchange.
  • aluminosilicates of the formula used Preferably aluminosilicates of the formula used.
  • the water bound in the aluminosilicates is also included in the water content of component (G).
  • the aluminosilicates have a particle size of less than 25 microns, with at least 80% by weight of the particles having a size of less than 10 microns.
  • aluminosilicates The proportion of aluminosilicates is 5 to 25% by weight, preferably 8 to 18% by weight, based on the anhydrous active substance.
  • Particularly suitable aluminosilicates are synthetic, finely divided zeolites of the NaA type and NaX type and their mixtures.
  • the ratio is preferably 1: 2 to 1: 3.5.
  • the sodium silicate content of the agents is 5 to 20% by weight, preferably 8 to 18% by weight and in particular 12 to 16% by weight. This information relates to anhydrous silicate.
  • the agents can contain sodium sulfate and / or sodium carbonate in amounts of up to 15% by weight, preferably not more than 10%. If component (F) consists of sodium sulfate, its proportion is generally 0.2 to 5% by weight. While components (C) to (E) are integrating components, which are important for both the grain properties and the cleaning effect, component (F) is ancillary and filler that does not significantly improve the product.
  • An essential component of the agent is the water content, which is a total of 5 to 12% by weight. Part of the water is comparatively firmly bound, for example as a component of the sodium aluminosilicate.
  • the proportion of water which can be removed at a drying temperature of 140 ° C. is preferably 4 to 8% by weight. This proportion is such that, on the one hand, there are no oxidative changes and browning, in particular no dust explosions, during spray drying, but on the other hand the desired grain properties, such as high strength, good flowability and low tendency to form lumps even under unfavorable conditions and a sufficiently high dissolution rate result. If these limits are clearly undershot, the oxidative changes increase; if they are significantly exceeded, the grain properties deteriorate in the sense of reduced strength and free-flowing properties.
  • organic chelating agents such as alkali metal salts of Aminoalkanpolyphosphonklaren or hydroxyalkane phosphonic acids, such as aminotrimethylenephosphonic acid, ethylenediaminetetramethylenephosphonic acid and 1-hydroxyethane-1,1-diphosphonic acids of aminopolycarboxylic acids such as nitrilotriacetic acid or ethylenediaminetetraacetic acid as well as the higher homologues of the polyacids mentioned.
  • Polymeric carboxylic acids which may optionally contain hydroxy ether and / or carbonyl groups, can also be used as complexing agents.
  • optical brighteners and anti-graying components which include, in particular, cellulose ethers, such as carboxyl methyl or methyl cellulose.
  • cellulose ethers such as carboxyl methyl or methyl cellulose.
  • the sum of all organic constituents including constituents (A) and (B) must be such that their proportion does not substantially exceed 50% by weight.
  • Another object of the invention is a process for the preparation of the compositions, characterized in that the aqueous containing 30 to 45 wt .-% Fried Slurry of components (A) to (F) atomized in a spray device, the drying gases carried in cocurrent or countercurrent having an inlet temperature of 150 ° to 350 ° C and an outlet temperature of 65 ° to 95 ° C.
  • the optional ingredients are also incorporated into the aqueous slurry and atomized.
  • Stabilized aluminosilicate suspensions of this type generally contain small amounts of stabilizing agents, for example nonionic surfactants or water-soluble polymers, which are incorporated into the end product in this way.
  • stabilizing agents for example nonionic surfactants or water-soluble polymers.
  • the content of such suspension stabilizers in the agents according to the invention is, however, in view of the small amounts used in the suspensions, generally well below 1% by weight, usually below 0.5% by weight.
  • the remaining components of the composition can be distributed without problems in the aqueous slurry, and they can also be used as a dry substance or - if the total water balance allows this - also as an aqueous paste.
  • the latter applies in many cases to the surfactants, in particular to the alkylbenzenesulfonate, which, for example can be incorporated into the aqueous batch as a sodium salt solution or as a free acid with the addition of the appropriate amount of sodium hydroxide.
  • Spraying is usually carried out under high pressure using nozzles.
  • Air and combustion gases which can be introduced directly into the tower, are the primary drying gases.
  • the drying gas can be conducted in cocurrent or countercurrent to the spray product; preferably one uses the countercurrent principle and introduces the drying gas tangentially into the drying tower, so that a cyclone-like flow arises.
  • the spray product obtained has an average particle size of 0.4 to 0.8 mm, the proportion of particles with a particle size of less than 0.1 mm being less than 10% by weight, in particular less than 5% by weight and a grain size over 1.2 mm is less than 5% by weight, in particular not more than 2% by weight. Portions deviating from this grain spectrum are expediently sieved out and can be returned to the aqueous batch.
  • the bulk density is in the range from 250 to 450 g / l, preferably from 300 to 400 g / l.
  • the spray-dried agents have a porous grain structure, which differs from conventional spray-dried heavy-duty or mild detergents by an increased grain strength, without the solution properties being impaired thereby.
  • Despite high levels of organic matter, explosive or combustible dusts do not form during normal processing. They are easy to pour and do not tend to form lumps.
  • the agents can be used as detergents without further additives. But it can also be done retrospectively, i.e. to the finished product, in addition to other common detergent ingredients such as anionic and / or nonionic synthetic surfactants, soap, skeletal salts, e.g. Phosphates, washing alkalis, e.g. Soda, as well as bleach ,. such as per-compound or active chlorine carrier in granular or powdery form, or in another form directly before or during the application.
  • common detergent ingredients such as anionic and / or nonionic synthetic surfactants, soap, skeletal salts, e.g. Phosphates, washing alkalis, e.g. Soda, as well as bleach ,. such as per-compound or active chlorine carrier in granular or powdery form, or in another form directly before or during the application.
  • the bulk weight was 320 g / l.
  • packages made of cardboard are evenly filled with the product up to the standard filling level, closed with a lid that can be attached and in a machine-driven vibrating machine under defined Conditions compressed by directional impacts, which results in a reproducible compression of the content.
  • the package is opened and fastened in a device that allows it to be poured out at defined tilting angles.
  • the packages can be shaken by means of a motorized impact device.
  • the amount of powder flowing out is collected in a measuring cylinder. The following ratings are given, with the given degrees indicating the position of the package:
  • the consumer registers grades 1 to 3 as very good to good, grade 4 as satisfactory and grades 5 and 6 as poor or unsatisfactory.
  • the determination of the powder gave the grade 4 immediately after the spray drying and the grade 3 after storage for 3 days.
  • test value was 30 g with freshly sprayed powder and 0 g after storage for 3 days.
  • last value is generally 10 to 60 g.
  • a beaker volume 500 cm
  • 200 ml of tap water (15 ° dH) tempered to 30 ° C are pumped with the help of a motorized stirrer, which is equipped with 4 agitator blades bent downwards at an angle of 30 °, with a constant number of revolutions of 700 RPM stirred.
  • the distance between the agitator blades and the bottom of the vessel is 2.5 cm.
  • 1 g of the sample is carefully poured into the stirring cone7, avoiding lumps.
  • the solution is poured through a tared sieve with a mesh size of 0.1 mm and a diameter of 7 cm and sucked off using a suction bottle. Remnants of substance remaining in the beaker are transferred onto the sieve using as little water as possible.
  • the sieve is weighed back in air after a drying time of 24 hours.
  • compositions of the following composition were produced (in the form of the Na salts):

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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)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
EP82111827A 1981-12-28 1982-12-20 Agents de lavage granulaires très moussants séchés par pulvérisation avec une stabilité élevée des granulations et procédé pour sa fabrication Expired EP0084657B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82111827T ATE18070T1 (de) 1981-12-28 1982-12-20 Starkschaeumendes, koerniges waschmittel mit erhoehter kornstabilitaet und verfahren zu dessen herstellung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19813151536 DE3151536A1 (de) 1981-12-28 1981-12-28 Starkschaeumendes, koerniges waschmittel mit erhoehter kornstabilitaet und verfahren zu dessen herstellung
DE3151536 1981-12-28

Publications (2)

Publication Number Publication Date
EP0084657A1 true EP0084657A1 (fr) 1983-08-03
EP0084657B1 EP0084657B1 (fr) 1986-02-19

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EP82111827A Expired EP0084657B1 (fr) 1981-12-28 1982-12-20 Agents de lavage granulaires très moussants séchés par pulvérisation avec une stabilité élevée des granulations et procédé pour sa fabrication

Country Status (4)

Country Link
US (1) US4524010A (fr)
EP (1) EP0084657B1 (fr)
AT (1) ATE18070T1 (fr)
DE (2) DE3151536A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0290209A1 (fr) * 1987-04-30 1988-11-09 Unilever Plc Matière sèche par atomisation pour des compositions détergentes
EP0219314A3 (en) * 1985-10-09 1988-11-09 The Procter & Gamble Company Granular detergent compositions having improved solubility
EP0220024A3 (en) * 1985-10-09 1988-11-09 The Procter & Gamble Company Granular detergent compositions having improved solubility
WO1993002168A1 (fr) * 1991-07-15 1993-02-04 The Procter & Gamble Company Procede de production d'une composition detergente contenant des particules de sulfate d'alkyle et des granules de base
WO1997032005A1 (fr) * 1996-02-26 1997-09-04 Unilever Plc Particules de detergent anionique

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT1180819B (it) * 1984-09-12 1987-09-23 Mira Lanza Spa Metodo di neutralizzazione della zeolite a mediante trattamento con a cidi forti del panello di filtrazione addizionato con un fludificante
DE3742043A1 (de) * 1987-12-11 1989-06-22 Hoechst Ag Verfahren zur herstellung von kristallinen natriumschichtsilikaten
CA2027518A1 (fr) * 1990-10-03 1992-04-04 Richard L. Tadsen Methode de preparation de compositions detergentes a haute densite, contenant des particules tensio-actives sensibles au ph
IL108500A (en) * 1994-01-31 1998-06-15 Zohar Detergent Factory Fatty alcohol sulphates in granular form and process for their preparation
GB9711350D0 (en) * 1997-05-30 1997-07-30 Unilever Plc Granular detergent compositions and their production
PL337039A1 (en) * 1997-05-30 2000-07-31 Unilever Nv Particulate granular detergent compositions
US9332776B1 (en) 2010-09-27 2016-05-10 ZoomEssence, Inc. Methods and apparatus for low heat spray drying
US8939388B1 (en) 2010-09-27 2015-01-27 ZoomEssence, Inc. Methods and apparatus for low heat spray drying
US9861945B1 (en) 2017-08-04 2018-01-09 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
US9993787B1 (en) 2017-08-04 2018-06-12 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
US10155234B1 (en) 2017-08-04 2018-12-18 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
WO2019028446A1 (fr) 2017-08-04 2019-02-07 ZoomEssence, Inc. Appareil et procédé de séchage par pulvérisation à très haut rendement
US10486173B2 (en) 2017-08-04 2019-11-26 ZoomEssence, Inc. Ultrahigh efficiency spray drying apparatus and process
US10569244B2 (en) 2018-04-28 2020-02-25 ZoomEssence, Inc. Low temperature spray drying of carrier-free compositions

Citations (4)

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Publication number Priority date Publication date Assignee Title
DE1792431A1 (de) * 1967-09-04 1971-11-11 Unilever Nv Verfahren zur Herstellung von Wasch- und Reinigungsmitteln
DE2742683A1 (de) * 1976-09-29 1978-03-30 Colgate Palmolive Co Abgepacktes, teilchenfoermiges waschmittel
GB2013707A (en) * 1978-02-01 1979-08-15 Unilever Ltd Preparation of Spray-Dryed Detergent Compositions
DE2844455A1 (de) * 1978-10-12 1980-04-24 Henkel Kgaa Phosphatfreies waschmittel und verfahren zu dessen herstellung

Family Cites Families (14)

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GB1355187A (en) * 1970-07-10 1974-06-05 Unilever Ltd Production of detergent compositions
US3985669A (en) * 1974-06-17 1976-10-12 The Procter & Gamble Company Detergent compositions
LU70752A1 (fr) * 1974-08-19 1976-08-19
US4169075A (en) * 1974-10-10 1979-09-25 Henkel Kommanditgesellschaft Auf Aktien Process for the production of powdery washing agents by spray-drying
GB1516848A (en) * 1974-11-13 1978-07-05 Procter & Gamble Ltd Detergent composition
AT356628B (de) * 1976-02-06 1980-05-12 Henkel Kgaa Verfahren zur herstellung waesseriger, zur weiterverarbeitung zu wasch- und reinigungs- mitteln geeigneter suspensionen von fein- teiligen, zum kationenaustausch befaehigten, noch gebundenes wasser enthaltenden wasser- unloeslichen silikaten
DE2615698A1 (de) * 1976-04-09 1977-10-20 Henkel & Cie Gmbh Stabile suspensionen wasserunloeslicher, zum binden von calciumionen befaehigter silikate und deren verwendung zur herstellung von wasch- und reinigungsmitteln
US4269722A (en) * 1976-09-29 1981-05-26 Colgate-Palmolive Company Bottled particulate detergent
US4351740A (en) * 1976-09-29 1982-09-28 Colgate Palmolive Company Bottled particulate detergent
JPS5919600B2 (ja) * 1976-12-23 1984-05-07 ライオン株式会社 粒状洗剤の製造法
US4180485A (en) * 1977-11-02 1979-12-25 The Procter & Gamble Company Spray-dried detergent compositions
DE2829165A1 (de) * 1978-07-03 1980-01-17 Henkel Kgaa Verfahren zur herstellung von alumosilikat-granulat
JPS5919597B2 (ja) * 1980-04-23 1984-05-07 ライオン株式会社 ゼオライト含有無燐粒状洗剤組成物
US4344871A (en) * 1981-03-23 1982-08-17 The Procter & Gamble Company Spray-dried aluminosilicate detergents containing silicate and metaborate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1792431A1 (de) * 1967-09-04 1971-11-11 Unilever Nv Verfahren zur Herstellung von Wasch- und Reinigungsmitteln
DE2742683A1 (de) * 1976-09-29 1978-03-30 Colgate Palmolive Co Abgepacktes, teilchenfoermiges waschmittel
GB2013707A (en) * 1978-02-01 1979-08-15 Unilever Ltd Preparation of Spray-Dryed Detergent Compositions
DE2844455A1 (de) * 1978-10-12 1980-04-24 Henkel Kgaa Phosphatfreies waschmittel und verfahren zu dessen herstellung

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0219314A3 (en) * 1985-10-09 1988-11-09 The Procter & Gamble Company Granular detergent compositions having improved solubility
EP0220024A3 (en) * 1985-10-09 1988-11-09 The Procter & Gamble Company Granular detergent compositions having improved solubility
EP0290209A1 (fr) * 1987-04-30 1988-11-09 Unilever Plc Matière sèche par atomisation pour des compositions détergentes
WO1993002168A1 (fr) * 1991-07-15 1993-02-04 The Procter & Gamble Company Procede de production d'une composition detergente contenant des particules de sulfate d'alkyle et des granules de base
WO1997032005A1 (fr) * 1996-02-26 1997-09-04 Unilever Plc Particules de detergent anionique
AU724105B2 (en) * 1996-02-26 2000-09-14 Unilever Plc Anionic detergent particles

Also Published As

Publication number Publication date
US4524010A (en) 1985-06-18
ATE18070T1 (de) 1986-03-15
DE3269269D1 (en) 1986-03-27
EP0084657B1 (fr) 1986-02-19
DE3151536A1 (de) 1983-07-07

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