EP0719852B1 - Verwendung einer Schmierölzusammensetzung - Google Patents

Verwendung einer Schmierölzusammensetzung Download PDF

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Publication number
EP0719852B1
EP0719852B1 EP95309479A EP95309479A EP0719852B1 EP 0719852 B1 EP0719852 B1 EP 0719852B1 EP 95309479 A EP95309479 A EP 95309479A EP 95309479 A EP95309479 A EP 95309479A EP 0719852 B1 EP0719852 B1 EP 0719852B1
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EP
European Patent Office
Prior art keywords
oil
lubricant oil
weight
parts
oil composition
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
EP95309479A
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English (en)
French (fr)
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EP0719852A3 (de
EP0719852A2 (de
Inventor
Shouzou Matsushita
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Tonen General Sekiyu KK
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Tonen General Sekiyu KK
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Publication of EP0719852A2 publication Critical patent/EP0719852A2/de
Publication of EP0719852A3 publication Critical patent/EP0719852A3/xx
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Publication of EP0719852B1 publication Critical patent/EP0719852B1/de
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/02—Petroleum fractions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M129/38—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
    • C10M129/40—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms monocarboxylic
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/08—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium containing a sulfur-to-oxygen bond
    • C10M135/10—Sulfonic acids or derivatives thereof
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/08—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic sulfur-, selenium- or tellurium-containing compound
    • C—CHEMISTRY; METALLURGY
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    • C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
    • C10M159/12—Reaction products
    • C10M159/20—Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products
    • C10M159/24—Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products containing sulfonic radicals
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    • C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
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    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/045—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
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    • C10M173/00—Lubricating compositions containing more than 10% water
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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    • C10M2203/102—Aliphatic fractions
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    • C10M2203/102—Aliphatic fractions
    • C10M2203/1025—Aliphatic fractions used as base material
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/104—Aromatic fractions
    • C10M2203/1045—Aromatic fractions used as base material
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/106—Naphthenic fractions
    • C10M2203/1065—Naphthenic fractions used as base material
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    • C10M2203/108—Residual fractions, e.g. bright stocks
    • C10M2203/1085—Residual fractions, e.g. bright stocks used as base material
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    • C10M2205/026—Butene
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    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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    • C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
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    • C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
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    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/22—Metal working with essential removal of material, e.g. cutting, grinding or drilling
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    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/01—Emulsions, colloids, or micelles

Definitions

  • the present invention relates to a lubricant oil composition. More specifically, the present invention relates to a lubricant oil which can be separated immediately after it is mixed into a water-soluble cutting fluid, to readily remove the resultant floating oil components in separation by means of oil skimmers and the like.
  • Cutting oils are grouped into water-insoluble cutting fluids produced by adding oils, extreme pressure agents or the like to mineral oils, and water-soluble cutting fluids comprising a base oil, a surfactant, an extreme pressure agent and an oily agent, which are used after dilution with water.
  • water-soluble cutting fluids have greater cooling effects that the fluids are widely used.
  • sliding face oil In cutting or grinding metal workpieces, use is made of a lubricant oil called sliding face oil on the sliding surface between a slider supporting a grinding plate such as a blade and a pedestal guiding surface, the sliding face oil being capable of moving the grinding plate in a smooth fashion even if friction is generated between the grinding plate and the workpiece to prevent stickslip phenomena.
  • stickslip preventive agents such as phosphate ester, fatty acids and fatty acid esters, are added to base oils so as to provide stickslip preventive properties.
  • an antioxidant e.g., a metal deactivator, an extreme pressure agent and a tackifier may be added to the sliding face.
  • a water-soluble cutting fluid When a water-soluble cutting fluid is used on cut or ground portions of a workpiece, the water-soluble cutting fluid after use is transferred into a reservoir tank together with a part of a leaked sliding face oil.
  • lubricant oils such as hydraulic-actuated oils and other tooling oils may frequently contaminate such water-soluble cutting fluids.
  • the water-soluble cutting fluids are separated from such lubricant oils to be recycled for use. Because water-soluble cutting fluids contain a large quantity of a surfactant, however, the lubricant oil contaminating the water-soluble cutting fluids forms emulsion, which often causes difficulty in separating the lubricant oil.
  • the lubricant oil contaminating the water-soluble cutting fluid markedly deteriorates the properties of the water-soluble cutting fluid thereby shortening the life and causing poor work environment due to an offensive odor through rot and so on. Therefore, the development of a lubricant oil, which can be separated immediately after its contamination into a water-soluble cutting fluid, has been expected.
  • GB-A-1 103 533 discloses lubricating oil compositions comprising neutral or basic alkaline earth metal sulphonates and oleic acid.
  • US-A-4 770 798 discloses anti-corrosion lubricating oil compositions comprising e.g. naphthenic acid, calcium salt of sulphonic acid and saturated fatty acid.
  • the object of the present invention is to provide a lubricant oil for use in combination with water-soluble cutting fluids, which can separate and float immediately after its contamination with said water-soluble cutting fluid without forming stable emulsion and which can be removed readily from the water-soluble cutting fluid by means of an oil skimmer and the like.
  • the present invention is a use of a lubricant oil in combination with a water-soluble cutting fluid said lubricant oil comprising a minor portion of a calcium sulfonate, barium sulfonate, or mixture therein being neutral or having a lower base number, and a straight chain univalent fatty acid having a specific number of the carbon atoms and a major portion of a base oil.
  • the lubricating oil composition has excellent properties of separating from water-soluble cutting fluids.
  • the present invention is to provide:
  • the kinematic viscosity of the base oil to be used in the lubricant oil composition of the present invention may be 10 to 500 mm 2 /s, preferably 30 to 70 mm 2 /s at 40°C. If the kinematic viscosity is less than 10 mm 2 /s at 40°C, stickslip may occur on a sliding surface during low-speed operation. If the kinematic viscosity exceeds 500 mm 2 /s at 40°C, the floating of the table may be problematic.
  • the viscosity index of the base oil to be used in the lubricant oil composition in accordance with the present invention may be preferably 50 to 150, more preferably 100 to 120. If the viscosity index is less than 50, the viscosity change of the lubricant oil composition by temperature is so large that a change in the frictional properties may possibly be brought about.
  • the viscosity stability above the viscosity index of 150 is not required under the lubricating conditions at a temperature from room temperature to 50°C for use.
  • the kinematic viscosity and viscosity index of the base oil can be determined according to JIS K 2283.
  • the base oil to be used in the lubricant oil composition of the present invention has an aromatic component content of 20 wt% or less and a pour point of -10°C or less. If the content of aromatic components exceeds 20 wt%, the lubricant oil composition may potentially swell sealing rubber. If the pour point exceeds -10°C, the pouring properties may get poor at lower temperatures.
  • the base oil to be used in the lubricant oil composition of the present invention may be selected appropriately from known mineral oils and synthetic oils, if such oils may satisfy the above requirements.
  • mineral oils include a raffinate produced by solvent purifying a lubricant raw material by using an aromatic extraction solvent such as phenol, furfural, n-methyl pyrrolidone; a hydrogenated oil produced by hydrogenation by means of hydrogenating catalysts such as cobalt and molybdenum on a carrier silica-alumina; or a mineral oil such as a lubricant distillate produced by isomerization of wax, including 60 Neutral Oil, 100 Neutral Oil, 150 Neutral Oil, 300 Neutral Oil, 500 Neutral Oil, bright stock and the like.
  • synthetic oils include for example poly ( ⁇ -olefin oligomer), lucant, polybutene, alkylbenzene, polyol ester, poly gylcol ester, dibasic acid ester, phosphate ester, silicone oil and the like. These base oils may be used singly or in combination with two or more thereof. Also, such mineral oils and such synthetic oils may be mixed together for use.
  • the calcium sulfonate and barium sulfonate include a calcium salt and barium salt of for example petroleum sulfonic acid of a molecular weight of 400 to 1200, or synthetic sulfonic acid such as alkylbenzene sulfonic acid, alkylnaphthalene sulfonic acid and the like.
  • Petroleum sulfonic acid is produced by purifying a petroleum distillate and sulfonating the distillate with fuming sulfuric acid, which may be neutralized into a desirable salt.
  • Alkylbenzene sulfonic acid and alkylnaphthalene sulfonic acid may be produced by alkylating benzene and naphthalene, respectively, and sulfonating the resulting products with fuming sulfuric acid, which may be then neutralized into desirable salts.
  • the calcium sulfonate(s) and barium sulfonate(s) may be used singly or used in combination with two or more thereof. If the total base number of a calcium sulfonate or barium sulfonate exceeds 100 mg KOH/g, the properties of the lubricant oil composition separating from a water-soluble cutting fluid may be deteriorated.
  • calcium sulfonate(s), barium sulfonate(s), or mixture thereof is blended preferably at a ratio of 0.01 to 5.0 parts by weight, more preferably 0.1 to 2.0 parts by weight to 100 parts by weight of the base oil. If the calcium sulfonate(s), barium sulfonate(s) or mixture thereof is (are) blended at an amount of less than 0.01 parts by weight to 100 parts by weight of the base oil, the properties of the lubricant oil composition separating from a water-soluble cutting fluid may possibly be deteriorated.
  • the properties of the lubricant oil composition separating from a water-soluble cutting fluid may not be improved in proportion to the increase of the amount of the calcium sulfonate or barium sulfonate to be blended.
  • straight chain univalent fatty acid(s) having 8 to 18 carbon atoms.
  • straight chain fatty acid(s) includes, for example, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, palmitoleic acid, oleic acid and the like. Even if the number of the carbon atoms of the straight chain fatty acid is either less than 8 or more than 18, the compatibility of the base oil with the straight chain fatty acid may be deteriorated potentially. Among them, myristic acid and palmitic acid are preferable.
  • the lubricant oil composition of the present invention is blended preferably 0.01 to 5.0 parts, more preferably 0.1 to 2.0 parts by weight of straight chain univalent fatty acid(s) having 8 to 18 carbon atoms to 100 parts by weight of the base oil. If straight chain univalent fatty acid(s) having 8 to 18 carbon atoms is blended at an amount of less than 0.01 parts by weight to 100 parts of the base oil, the properties of the lubricant oil composition separating from the water-soluble cutting fluid may possibly be deteriorated.
  • additives conventionally used in lubricant oils such as antioxidants, wear preventive agents, friction adjusters, metal deactivators, extreme pressure agents, rust preventives, adhesion improving agents and the like, may be added to the lubricant oil composition of the present invention.
  • antioxidants use may be made of, for example, phenol series antioxidants, sulfur-containing antioxidants, nitrogen-containing antioxidants and the like, singly or in combination therewith.
  • phenol series antioxidants use may be made of 2,6-di-t-butyl-p-cresol, 2,6-di-t-butylphenol, 4,4'-methylene bis(2,6-di-t-butylphenol) and the like;
  • sulfur-containing antioxidants use may be made of diphenyl monosulfide, diphenyl disulfide and the like;
  • nitrogen-containing antioxidants use may be made of alkylated diphenylamine, phenyl- ⁇ -naphthylamine, alkylated ⁇ -naphthylamine, and the like.
  • Such wear preventive agents include for example dibenzyl disulfide, polysulfide, sulfurized fat and oil, sulfide ester, phosphate ester, phosphite ester, thiophosphate ester, zinc thiophosphate, zinc thiocarbamate and the like.
  • Such friction adjusters include for example polyhydric alcohol partial ester, amine, amide, sulfide ester, sulfurized fat and oil, phosphate ester, phosphate ester amine salt, phosphite ester and organic molybdenum compounds and the like.
  • Such metal deactivators include for example 2,5-dimercapto-1,3,4-thiadiazole and benzotriazole series and the like.
  • Such extreme pressure agents include for example olefin sulfide.
  • Such rust preventives include for example dinonyl naphthalene calcium sulfonate basic salt, dinonyl naphthalene barium sulfonate basic salt and the like.
  • Such viscosity index improving agents include for example polymethacrylate series, polyisobutylene series, ethylene-propylene copolymer series, styrene-butadiene hydrogenation copolymer series and the like.
  • the aforementioned additives may be blended at a ratio of 0.01 to 5.0 parts by weight to 100 parts by weight of the base oil.
  • the lubricant oil composition of the present invention exerts the extremely great separation properties when used in combination with a cutting fluid prepared by diluting a water-soluble cutting fluid with water.
  • the water-soluble cutting fluid defined by JIS K2241 includes an emulsion type, soluble type and chemical solution type.
  • the lubricant oil composition of the present invention has excellent separation properties for any of the types.
  • a cutting fluid use was made of a commercially available emulsion-type water-soluble cutting fluid (manufactured by Yushio Chemical Co., Ltd.) thirtyfold diluted with ion exchanged water.
  • the cutting fluid and a simple lubricant oil were weighed and picked up into a test tube such that the cutting fluid and sample lubricant oil were 40 ml in volume, respectively, at the test temperature.
  • the test tube was placed and held in a constant temperature bath kept at the test temperature.
  • a stirring plate was placed in the center of the test tube to stir up at the rate of 1500 ⁇ 15 revolutions per minute for just 5 minutes. After the completion of stirring, the inside of the test tube was observed from the side face to record the volumes of the oil layer, the cutting fluid layer, and the emulsified layer every 10 minutes over 60 minutes. All the kinematic viscosities of the sample lubricant oils prepared in the present Examples and Comparative Examples were within 28.8 to 90 mm 2 /s at 40°C. The test temperature was set at 54 ⁇ 1°C.
  • a sample lubricant oil was prepared by blending 0.2 parts by weight of di-t-butyl-p-cresol as an antioxidant, 0.5 parts by weight of dibenzyl disulfide as a wear preventive agent, 2 parts by weight of the salt of di-iso-octyl phosphate and monotetradecylamine as a friction adjuster, 0.5 parts by weight of calcium sulfonate (neutral salt) and 0.3 parts by weight of palmitic acid, to 100 parts by weight of a mineral oil series base oil having a kinematic viscosity of 68.0 mm 2 /s at 40°C.
  • sample lubricant oil compositions were prepared to carry out the demulsibility test. The results are shown in Table 1.
  • each of an oil layer and a cutting fluid layer is separated by 30 ml or more in the course of 60 minutes, so that the lubricant oil is regarded as practically having excellent separation properties though the properties are inferior to those of the lubricant oils of Examples 1 to 4.
  • the lubricant oil of Comparative Example I blended with palmitic acid and no sulfonate does not separate an oil layer in the course of 60 minutes.
  • the lubricant oil of Comparative Example 2 blended with a calcium sulfonate (neutral salt) and no straight chain fatty acid both of an oil layer and a cutting fluid do fall short of 30 ml in volume even in the course of 60 minutes.
  • the lubricant oil composition of the present invention exerts excellent separation properties from a cutting fluid prepared by diluting a water-soluble cutting fluid. Therefore, the composition so readily separates and floats in a reservoir tank for the cutting fluid that the composition can be removed simply by means of an oil skimmer and the like. Thus, the properties of the water-soluble cutting fluid can be maintained for a long term, with no occurrence of poor work environment due to rot and so on.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Lubricants (AREA)

Claims (7)

  1. Verwendung einer Schmierölzusammensetzung in Kombination mit wasserlöslichen Schneidflüssigkeiten, wobei die Schmierölzusammensetzung einen geringeren Anteil Calciumsulfonat(e), Bariumsulfonat(e) oder Mischung davon, die neutral ist bzw. sind oder die Gesamtbasenzahl von 100 mg KOH/g oder weniger hat bzw. haben, und geradkettige(n) einwertige(n) Fettsäure(n) mit 8 bis 18 Kohlenstoffatomen und einen größeren Anteil Basisöl der Mineralreihen und/oder synthetischen Ölreihen umfasst, wobei das Basisöl eine kinematische Viskosität von 10 bis 500 mm2/s bei 40°C hat.
  2. Verwendung einer Schmierölzusammensetzung nach. Anspruch 1, wobei die Schmierölzusammensetzung 0,001 bis 5,0 Gewichtsteile Calciumsulfonat(e), Bariumsulfonat(e) oder Mischung davon auf 100 Gewichtsteile des Basisöls enthält.
  3. Verwendung nach Anspruch 1 oder 2, wobei die geradkettige(n) einwertige(n) Fettsäure(n) in einer Menge von 0,01 bis 5,0 Gewichtsteilen auf 100 Gewichtsteile des Basisöle in die Zusammensetzung gemischt wird bzw. werden.
  4. Verwendung nach einem der vorhergehenden Ansprüche, wobei die kinematische Viskosität des Basisöls bei 40°C 30 bis 70 mm2/s beträgt.
  5. Verwendung nach einem der vorhergehenden Ansprüche, wobei der Viskositätsindex des Basisöls 50 bis 150 ist.
  6. Verwendung nach einem der vorhergehenden Ansprüche, wobei das Basisöl 20 Gew.-% oder weniger Aromaten enthält.
  7. Verwendung nach einem der vorhergehenden Ansprüche, wobei die Gesamtbasenzahl von Calciumsulfonat(en), Bariumsulfonat(en) oder Mischung davon 50 mg KOH/g oder weniger ist.
EP95309479A 1994-12-28 1995-12-22 Verwendung einer Schmierölzusammensetzung Expired - Lifetime EP0719852B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP339601/94 1994-12-28
JP6339601A JPH08183980A (ja) 1994-12-28 1994-12-28 潤滑油組成物
JP33960194 1994-12-28

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EP0719852A2 EP0719852A2 (de) 1996-07-03
EP0719852A3 EP0719852A3 (de) 1996-07-31
EP0719852B1 true EP0719852B1 (de) 2005-11-23

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JPH09328698A (ja) * 1996-04-10 1997-12-22 Nippon Oil Co Ltd すべり案内面用潤滑油組成物
JP3261340B2 (ja) * 1997-05-30 2002-02-25 東燃ゼネラル石油株式会社 潤滑油組成物
WO2023008545A1 (ja) * 2021-07-30 2023-02-02 出光興産株式会社 熱処理油組成物

Citations (1)

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Publication number Priority date Publication date Assignee Title
US4770798A (en) * 1984-04-13 1988-09-13 Labofina, S.A. Lubricating and anti-corrosion compositions

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SE308766B (de) * 1965-06-17 1969-02-24 Gulf Research Development Co
DE2854975C2 (de) * 1978-12-20 1986-08-07 Hoechst Ag, 6230 Frankfurt Emulsionsspalter
SU1198110A1 (ru) * 1984-06-01 1985-12-15 Институт черной металлургии Способ регенерации масла из пенных отходов смазочно-охлаждающих жидкостей

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4770798A (en) * 1984-04-13 1988-09-13 Labofina, S.A. Lubricating and anti-corrosion compositions

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DE69534628T2 (de) 2006-08-10
EP0719852A3 (de) 1996-07-31
CA2165868A1 (en) 1996-06-29
ES2253743T3 (es) 2006-06-01
JPH08183980A (ja) 1996-07-16
SG50391A1 (en) 1998-07-20
CA2165868C (en) 2006-10-31
EP0719852A2 (de) 1996-07-03
DE69534628D1 (de) 2005-12-29

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