EP0500951A1 - Composition detergente sans halogene - Google Patents

Composition detergente sans halogene Download PDF

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Publication number
EP0500951A1
EP0500951A1 EP91915268A EP91915268A EP0500951A1 EP 0500951 A1 EP0500951 A1 EP 0500951A1 EP 91915268 A EP91915268 A EP 91915268A EP 91915268 A EP91915268 A EP 91915268A EP 0500951 A1 EP0500951 A1 EP 0500951A1
Authority
EP
European Patent Office
Prior art keywords
composition
alcohol
formula
alkylene oxide
alcohol solvent
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.)
Withdrawn
Application number
EP91915268A
Other languages
German (de)
English (en)
Other versions
EP0500951A4 (fr
Inventor
Kenichiro Nagata
Noboru 373 Horiikecho Yamashita
Shizuo Nishiyama
Giichi Akazome
Koichi Murai
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.)
New Japan Chemical Co Ltd
Original Assignee
New Japan Chemical Co Ltd
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 JP2231058A external-priority patent/JPH0826347B2/ja
Priority claimed from JP26718690A external-priority patent/JPH04142399A/ja
Priority claimed from JP22827291A external-priority patent/JPH0543896A/ja
Priority claimed from JP22827191A external-priority patent/JPH0543895A/ja
Application filed by New Japan Chemical Co Ltd filed Critical New Japan Chemical Co Ltd
Publication of EP0500951A1 publication Critical patent/EP0500951A1/fr
Publication of EP0500951A4 publication Critical patent/EP0500951A4/xx
Withdrawn legal-status Critical Current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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/26—Organic compounds containing oxygen
    • C11D7/261—Alcohols; Phenols
    • 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
    • C11D3/43—Solvents
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/50—Solvents
    • C11D7/5004—Organic solvents
    • C11D7/5013—Organic solvents containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
    • C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/26—Organic compounds containing oxygen
    • C11D7/266—Esters or carbonates
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/26—Organic compounds containing oxygen
    • C11D7/267—Heterocyclic compounds
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C11D7/3227—Ethers thereof

Definitions

  • the present invention relates to an alcohol-based, halogen-free cleaning composition effective for removing oils, rosin-based fluxes, adhesives, waxes and the like which are deposited on electronic parts, the surfaces of various metals and plastics, textile materials and the like.
  • Flons have many excellent properties such that they are low in toxicity, incombustible, chemically stable, do not erode the materials to be cleaned such as plastics materials and the like, maintain a strong permeation, are quick-drying, etc., and therefore flons have been heretofore employed in wide fields such as refrigerants for air conditioners and refrigerators, propellants for sprays, blowing agents for heat insulating materials such as urethane foam and the like and cleaning agents for electric and electronic parts, precision machines and the like.
  • the present inventors conducted extensive research in order to develop a cleaning composition which has excellent properties as achieved by the conventional flon-based cleaning agents such as high cleaning ability, chemical stability and the like and which contains in no way chlorine, fluorine and like halogen, is free from the possibility of destroying the natural environment and is further improved in cleaning properties.
  • the present inventors found that, by using aliphatic or alicyclic alcohols having a specific structure or the derivative thereof as a solvent component and adding thereto a predetermined quantity of a specific cyclohexylamine compound, it is possible to obtain a cleaning composition which is pronouncedly improved in cleaning properties as compared with the case where the foregoing solvent component is used alone, and which is suitable for dissolving and removing more general kinds of substances, namely applicable to a wider variety of technical fields.
  • the present inventors further found that an aqueous composition prepared by adding water to the cleaning composition obtained above has outstanding properties such that said aqueous composition is less flammable, is suppressed in irritant action, is thus improved in safety during operation and the like.
  • this composition is a cleaning composition which serves to sufficiently achieve the aforementioned object, i.e. which can replace flon-based cleaning agents.
  • the present invention has been accomplished based on these novel findings.
  • the present invention provides a halogen-free cleaning composition comprising a mixture of:
  • Such acetate compounds are known compounds or can be prepared with ease by a known process.
  • Specific examples of such acetate compound are ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol monopropyl ether acetate, ethylene glycol monoisopropyl ether acetate, ethylene glycol monobutyl ether acetate, ethylene glycol diacetate, diethylene glycol monomethyl ether acetate, diethylene glycol monoethyl ether acetate, diethylene glycol monopropyl ether acetate, diethylene glycol monoisopropyl ether acetate, diethylene glycol monobutyl ether acetate, triethylene glycol monomethyl ether acetate, triethylene glycol monoethyl ether acetate, propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, propylene glycol monopropyl ether acetate, propy
  • ethylene glycol monomethyl ether acetate particularly preferred are ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol diacetate, diethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether acetate, dipropylene glycol monomethyl ether acetate, or mixtures of these compounds.
  • the foregoing alcohol solvents (1) to (4) are each usable singly or at least two of them can be used in mixture.
  • a cleaning composition comprising the adduct of aliphatic alcohol with alkylene oxide represented by the formula (3) as an essential component.
  • A is as defined above in the formula (1), and q is an integer of 1 to 3.
  • cyclohexylamine compound examples include adducts of cyclohexylamine with EO, with PO or with a mixture of EO and PO. These compounds are each usable singly or at least two of them can be used in combination. These compounds are known compounds or can be readily prepared by a conventional method, e.g. by adding to cyclohexylamine a specified quantity of alkylene oxide with heating and under normal or elevated pressure using a basic catalyst such as caustic alkali, sodium methoxide or the like. When, among the cyclohexylamine compounds, an EO adduct of cyclohexylamine is used, a cleaning composition having an excellent dissolving power can be obtained.
  • Addition of cyclohexylamine with alkylene oxide serves to elevate the boiling point to improve the safety of the cleaning composition, and further serves to diminish the odor peculiar to cyclohexylamine, whereby the work environment can be improved.
  • the number of moles of the alkylene oxide to be added is about 1 to about 6 moles.
  • the cyclohexylamine compound of the formula (5) is used in an amount of about 0.1 to about 30 parts by weight, preferably about 1 to about 15 parts by weight, per 100 parts by weight of at least one of the above alcohol solvents (1) to (4).
  • Use of the cyclohexylamine compound in an amount less than 0.1 part by weight tends to impair the ability of the resulting cleaning composition to dissolve the substance to be removed by cleaning.
  • Even if the cyclohexylamine compound is used in an amount more than 30 parts by weight remarkably improved effects can not be produced, resulting in an economical disadvantage, and, with regard to some kinds of articles to be cleaned, e.g. surface-treated electronic parts and the like, there arises a tendency of swelling the surface-protecting film present on the surface of the article to be cleaned as well as the substance to be removed by cleaning.
  • the cleaning composition according to the invention can be used as a non-aqueous composition consisting essentially of an active ingredient, i.e. a mixture of at least one member of the foregoing alcohol solvents (1) to (4) and the cyclohexylamine compound of the formula (5).
  • an aqueous cleaning composition can be prepared by mixing said mixture with water.
  • aqueous cleaning composition is in the form of an aqueous solution or an aqueous emulsion, but is usually in the form of an aqueous solution.
  • the amount of water to be used can be suitably determined according to the intended use.
  • the aqueous composition is made into an aqueous solution containing the mixture at a concentration of at least 2% by weight but less than 100% by weight, preferably about 10 to about 80% by weight.
  • the aqueous cleaning composition obtained in this way is not deteriorated in cleaning ability and is non-flammable, thus improving the safety from the environmental and operation viewpoints.
  • the amount of the mixture is not limited to the above range insofar as the desired effects can be achieved.
  • the cleaning composition according to the invention by using at least one member of the above alcohol solvents of the formulas (1) to (4) in combination with a specific quantity of the cyclohexylamine compound of the formula (5), the components synergically act, and improve permeation property and ability to dissolve the substances to be removed by cleaning as compared with the case where each component is used singly, thus pronouncedly improving the cleaning performance.
  • the cleaning composition of the present invention may have incorporated therein additives conventionally used in the art such as anti-oxidizing agent, mildewproofing agent, rust preventive, anti-foaming agent and the like.
  • the thus obtained cleaning composition of the present invention is capable of dissolving well fats and oils, mineral oil, silicone oil, waxes, rosin-based fluxes, paraffinic adhesives, rosin-based adhesives and the like and only a small quantity of ionic residual substances remain.
  • the cleaning composition of the invention is usable in the fields in which flon-based cleaning compositions have been conventionally used, namely the cleaning composition of the invention is most suitable for removing organic oils adhered to printed circuit boards, ceramic element, condensers, liquid crystal display devices and like electronic parts, brushes, rotors and like electric parts, bearings, chips and like parts of precision machines, parts of optical instruments used for cameras, glasses and the like, parts for motor vehicles, etc.
  • the kind of the material of the article to be cleaned is not specifically limited.
  • examples of such material are metals, plastics, elastomer and composite materials thereof, etc.
  • the composition of the invention is applicable to a wide range of fields in which not only flon-based cleaning agents but also other halogen-based cleaning agents have been hitherto used (for example, cleaning agents for laundry, etc.).
  • the cleaning can be conducted by bringing the non-aqueous or aqueous cleaning composition of the invention into contact with the substance to be removed from the article to be cleaned.
  • the article to be cleaned is immersed in the cleaning composition maintained at a temperature of around room temperature to about 80°C for about 1 minute to about several hours to swell the dirt when so required, or the cleaning liquid is stirred, rocked or subjected to supersonic vibration (for about 10 seconds to about 1 hour), or subjected to a combination of these procedures under the foregoing temperature condition for removing the dirt.
  • the article is washed with water or rinsed with a lower alcohol having 1 to 4 carbon atoms to remove the remaining cleaning composition, followed by drying.
  • the present invention also provides a method for cleaning the surface of an article which is soiled with an organic substance such as the aforementioned fats and oils, mineral oil, silicone oil, waxes, rosin-based fluxes, paraffinic adhesives, rosin-based adhesives or the like, the method being characterized in that the non-aqueous or aqueous cleaning composition of the invention is brought into contact, with the article to be cleaned.
  • an organic substance such as the aforementioned fats and oils, mineral oil, silicone oil, waxes, rosin-based fluxes, paraffinic adhesives, rosin-based adhesives or the like
  • the halogen-free cleaning composition according to the present invention has the following excellent properties, and can replace the conventional flon-based cleaning agents.
  • a cleaning composition having the formulation as shown below in Table 1.
  • the composition was maintained at 60°C with stirring.
  • a test piece 50 x 15 mm
  • a test piece made of a copper plate to which a mineral oil was adhered was cleaned by immersing the test piece in the cleaning composition for 15 minutes with stirring. After the cleaning, the test piece was washed with water for 5 minutes and then dried at 105°C for 30 minutes.
  • Each of the cleaning compositions as shown in Table 2 was placed into a cleaning chamber of an ultrasonic cleaner (trade name "THREE WAVE ULTRASONIC CLEANER SUS-103", product of Shimadzu Rika Instrument K.K.), and the composition was maintained at 60°C.
  • Electronic parts a laminate of chips made of glass to which a paraffinic adhesive was adhered were immersed in the composition and cleaned by using multi-ultrasonic wave (repeated use of waves having wavelengths of 28, 45 and 100 KHz for 30 seconds, the same applies hereinafter) for 10 minutes.
  • the chips thus cleaned were then washed with water for 5 minutes, rinsed with ethanol and dried at 80°C for 1 hour.
  • Each of the cleaning compositions having the formulation as shown below in Table 3 was placed into the cleaning chamber of the same type of ultrasonic cleaner as used in Example 6, and the composition was maintained at 60°C.
  • An electronic element to which a rosin-based solder flux was adhered was immersed in the composition and subjected to ultrasonic cleaning for 5 minutes using ultrasonic waves of multi-wavelengths. Thereafter, the element was washed with water, rinsed with ethanol and dried at 80°C for 1 hour.
  • a cleaning composition having the formulation as shown below in Table 4 was placed into a cleaning chamber of the same type of cleaner as employed in Example 6 and the composition was maintained at 25°C.
  • An electronic element to which silicone oil was adhered was immersed in the cleaning composition and was subjected to ultrasonic cleaning for 10 seconds using ultrasonic waves of multi-wavelengths. Thereafter, the element was washed with water, rinsed with ethanol and dried at 80°C for 1 hour.
  • Each of the cleaning compositions having the formulation as shown below in Table 5 was placed into the cleaning chamber of the same type of cleaner as employed in Example 6 and the composition was maintained at 70°C.
  • An electronic element to which a wax was adhered was immersed in the composition and subjected to ultrasonic cleaning for 5 minutes using ultrasonic waves of multi-wavelengths. The element was then washed with water, rinsed with ethanol and dried at 80°C for 1 hour.
  • a cleaning composition having the formulation as shown below in Table 6 was placed into the cleaning chamber of the same type of cleaner as used in Example 6 and the composition was maintained at 80°C.
  • Electronic parts made of glass (a laminate of chips) to which a rosin-based adhesive was adhered were immersed in the composition for 30 minutes and then subjected to ultrasonic cleaning for 10 minutes using ultrasonic waves of multi-wavelengths. The electronic part was thereafter washed with water for 5 minutes, rinsed with ethanol and dried at 80°C for 1 hour.

Abstract

L'invention se rapporte à une composition détergente sans halogène, qui comprend: (a) 100 parties en poids d'au moins un solvant à l'alcool choisi dans le groupe constitué par l'alcool tétrahydrofurfurylique et par des produits d'addition d'oxyde d'alkylène de cet alcool, par des alcools aliphatiques, par des produits d'addition d'oxyde d'alkylène de ces alcools et par des acétates de ces produits d'addition, ainsi que (b) environ 0,1 à 30 parties en poids d'un mélange de composés de cyclohexylamine représentés par la formule générale (5), où X et Y, qui peuvent être identiques ou différents entre eux, représentent chacun hydrogène ou -(AO)qH, à condition que X et Y ne représentent pas des atomes d'hydrogène en même temps; A représente alkylène C2 à C3; et q est égal à un nombre entier compris entre 1 et 3.
EP91915268A 1990-08-31 1991-08-28 Composition detergente sans halogene Withdrawn EP0500951A1 (fr)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
JP2231058A JPH0826347B2 (ja) 1990-08-31 1990-08-31 非塩素系洗浄剤組成物
JP231058/90 1990-08-31
JP26718690A JPH04142399A (ja) 1990-10-03 1990-10-03 非ハロゲン系洗浄剤組成物
JP267186/90 1990-10-03
JP22827291A JPH0543896A (ja) 1991-08-12 1991-08-12 非ハロゲン系洗浄剤組成物
JP22827191A JPH0543895A (ja) 1991-08-12 1991-08-12 非ハロゲン系洗浄剤組成物
JP228271/91 1991-08-12
JP228272/91 1991-08-12

Publications (2)

Publication Number Publication Date
EP0500951A1 true EP0500951A1 (fr) 1992-09-02
EP0500951A4 EP0500951A4 (fr) 1994-02-02

Family

ID=27477317

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91915268A Withdrawn EP0500951A1 (fr) 1990-08-31 1991-08-28 Composition detergente sans halogene

Country Status (3)

Country Link
EP (1) EP0500951A1 (fr)
KR (1) KR927003781A (fr)
WO (1) WO1992004436A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5456853A (en) * 1993-04-23 1995-10-10 Rust-Oleum Corporation Paint stripping composition based on tetrahydrofurfuryl alcohol and oxygenated aliphatic solvents
DE4436425A1 (de) * 1994-10-12 1996-04-18 Wack O K Chemie Gmbh Verfahren zur Reinigung von polierten Metallflächen
DE19545676A1 (de) * 1995-12-07 1997-06-12 Wack O K Chemie Gmbh Verfahren zum Aktivieren von Leiterplatinen
WO2017190206A1 (fr) * 2016-05-05 2017-11-09 Oxiteno S.A. Indústria E Comércio Composition solvante pour produits de nettoyage de surface et formulation pour produit de nettoyage de surface
US11008537B2 (en) 2016-03-03 2021-05-18 Lg Chem, Ltd. Cleaning composition for liquid crystal alignment layer and manufacturing method of liquid crystal alignment layer using the same

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63168498A (ja) * 1986-12-29 1988-07-12 ユシロ化学工業株式会社 床用つや出し剤除去用の洗浄剤

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6356580A (ja) * 1986-08-26 1988-03-11 Dai Ichi Kogyo Seiyaku Co Ltd 水切り乾燥用添加剤
JPS63110297A (ja) * 1986-10-27 1988-05-14 ユシロ化学工業株式会社 床用洗浄剤
JPS63112699A (ja) * 1986-10-31 1988-05-17 ユシロ化学工業株式会社 床用洗浄剤
JPS63121685A (ja) * 1986-11-07 1988-05-25 Dai Ichi Kogyo Seiyaku Co Ltd 洗浄剤

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63168498A (ja) * 1986-12-29 1988-07-12 ユシロ化学工業株式会社 床用つや出し剤除去用の洗浄剤

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Derwent Publications Ltd., London, GB; AN 88-232908 & JP-A-63 168 498 (YUSHIRO KK) 12 July 1988 *
See also references of WO9204436A1 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5456853A (en) * 1993-04-23 1995-10-10 Rust-Oleum Corporation Paint stripping composition based on tetrahydrofurfuryl alcohol and oxygenated aliphatic solvents
DE4436425A1 (de) * 1994-10-12 1996-04-18 Wack O K Chemie Gmbh Verfahren zur Reinigung von polierten Metallflächen
DE19545676A1 (de) * 1995-12-07 1997-06-12 Wack O K Chemie Gmbh Verfahren zum Aktivieren von Leiterplatinen
US11008537B2 (en) 2016-03-03 2021-05-18 Lg Chem, Ltd. Cleaning composition for liquid crystal alignment layer and manufacturing method of liquid crystal alignment layer using the same
WO2017190206A1 (fr) * 2016-05-05 2017-11-09 Oxiteno S.A. Indústria E Comércio Composition solvante pour produits de nettoyage de surface et formulation pour produit de nettoyage de surface

Also Published As

Publication number Publication date
WO1992004436A1 (fr) 1992-03-19
KR927003781A (ko) 1992-12-18
EP0500951A4 (fr) 1994-02-02

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