EP0711337A1 - Peroxyacides ou leurs precurseurs utilisables dans le nettoyage des textiles, et procedes de nettoyage de textiles a l'aide de ces peroxyacides ou de leurs precurseurs - Google Patents

Peroxyacides ou leurs precurseurs utilisables dans le nettoyage des textiles, et procedes de nettoyage de textiles a l'aide de ces peroxyacides ou de leurs precurseurs

Info

Publication number
EP0711337A1
EP0711337A1 EP94926403A EP94926403A EP0711337A1 EP 0711337 A1 EP0711337 A1 EP 0711337A1 EP 94926403 A EP94926403 A EP 94926403A EP 94926403 A EP94926403 A EP 94926403A EP 0711337 A1 EP0711337 A1 EP 0711337A1
Authority
EP
European Patent Office
Prior art keywords
phase
water
washing
acid
sudsing
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Withdrawn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
EP94926403A
Other languages
German (de)
English (en)
Inventor
Petrus Joseph Lemaire
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.)
STICHTING INSTITUUT VOOR REINIGINGSTECHNIEKEN TNO
Original Assignee
STICHTING INSTITUUT VOOR REINIGINGSTECHNIEKEN TNO
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 STICHTING INSTITUUT VOOR REINIGINGSTECHNIEKEN TNO filed Critical STICHTING INSTITUUT VOOR REINIGINGSTECHNIEKEN TNO
Publication of EP0711337A1 publication Critical patent/EP0711337A1/fr
Withdrawn legal-status Critical Current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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3905—Bleach activators or bleach catalysts
    • C11D3/3907—Organic 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3945—Organic per-compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06F—LAUNDERING, DRYING, IRONING, PRESSING OR FOLDING TEXTILE ARTICLES
    • D06F31/00—Washing installations comprising an assembly of several washing machines or washing units, e.g. continuous flow assemblies
    • D06F31/005—Washing installations comprising an assembly of several washing machines or washing units, e.g. continuous flow assemblies consisting of one or more rotating drums through which the laundry passes in a continuous flow
    • 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
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/40—Specific cleaning or washing processes
    • C11D2111/44—Multi-step processes

Definitions

  • the present invention relates to the cleaning of textile by means of wet cleaning processes, in particular industrial laundering processes.
  • the object of wet cleaning is to remove dirt and stains and to clear the laundry of microorganisms and materials giving the laundry an unpleasant smell.
  • the kinds of dirt occurring in textile can be subdivided into water-soluble dirt and water-insoluble dirt that partly consists of suspendable or emulsifiable dirt.
  • Water-soluble dirt comprises, e.g., sugars, acids, salts, and urea;
  • water-insoluble dirt comprises, e.g., sand, clAy, proteins, fats, oils, soot, dyes, and microorganisms.
  • Suspendable and emulsifiable dirt comprises, inter alia, proteins, starch, foods, fats, oils, and blood constituents.
  • the invention particularly relates to wet cleaning processes carried out in a so-called washing tube or washing line.
  • a washing tube is a (semi)continuous washing equipment comprising a number of successive chambers. In the different chambers different phases of the washing process are carried out, of which a phase can extend over more than one chamber.
  • the phases (see Fig. 1) of such a wet cleaning process mostly comprise a soaking phase, one or more sudsing phases, a rinsing phase, a bleaching phase, and a neutralization phase.
  • the dirty laundry is contacted with water and a detergent so that the dirt can swell.
  • the actual washing step takes place in the sudsing phase in which washing is carried out at a temperature of about 85°C in the presence of a washing agent.
  • washing agent and detached dirt are rinsed out.
  • Bleaching agent is added in the bleaching phase in order to oxidize and/or discolor soils that cannot be washed out.
  • residues of washing agent and bleaching agent are neutralized and rinsed out.
  • the different phases of the washing process are spatially separated in a washing tube (see Fig. 2) .
  • the figure shows a conventional washing tube. In chambers l through 3 soaking takes place.
  • the sudsing phase is carried out in chambers 4 through 8. In this phase it is possible to supply steam at different places to increase the sudsing temperature.
  • the process is carried out partly in countercur ent.
  • the waste water is discharged into chamber 4.
  • the sudsing phase is followed by the rinsing phase which is generally also carried out in countercurrent.
  • the rinsing phase is followed by the bleaching phase in which hitherto hypochlorite solutions are generally used, in particular in processes for cleaning white laundry and wash- fast and chlorine-fast colored laundry.
  • the last phase is the neutralization phase in which basic washing agent residues and hypochlorite are mostly neutralized by means of sodium hydrogen sulfite (bisulfite) .
  • the hydrogen peroxide process peroxide, instead of hypochlorite, is added in a second sudsing phase. In this case there is no separate bleaching phase.
  • the bleaching agents and/or disinfecting agents hitherto used particularly' in combination with the conventional neutralization by means of sulfite, have a number of drawbacks.
  • Dye stains and burned-in proteinic stains can only be removed by means of a bleaching treatment or a treatment with hot caustic soda.
  • bleaching is carried out with a sodium hypochlorite solution at a pH of about 9.5-11 and at a temperature of 25°C.
  • the active chlorine concentration is about 0.25 g/1 at a bleaching time of about 10 minutes.
  • a higher temperature gives too much chemical wear.
  • the use of perborate and/or hydrogen peroxide requires a higher temperature (>60°C) in order to obtain a somewhat bleaching action.
  • the above-described bleaching agents also have a somewhat disinfecting action, although the disinfecting action of peroxide is not great.
  • the procedures according to the prior art cannot prevent the reinfection of the textile with microorganisms in the last phases of the washing process because the disinfecting agent must be completely neutralized.
  • hypochlorite complete neutralization is necessary because strong chemical wear occurs in the presence of residues of active hypochlorite in the laundry or the water to be fed back to the process.
  • the water consumption of a washing tube is no less than 13 1 (including steam) per kg of laundry.
  • hypochlorite process see Fig. 2
  • this can be done with water after the neutralization phase, which may be reused in the soaking phase; and with water after the sudsing phase which can be used again in the soaking phase and/or sudsing phase.
  • water after the first sudsing phase can be added again to the beginning of the first sudsing phase, ithout the present invention this is the most feasible reuse of process water.
  • hypochlorite or hydrogen peroxide process water must be added again with care because, e.g., the water to be fed back to the soaking bath is warmer than is conventional in the soaking phase and that in the presence of residual hydrogen peroxide fixation of proteinic stains occurs, while in the case of hypochlorite a strong bleaching action and therefore chemical damage to the textile occurs owing to the increased tenperature.
  • the present invention provides a process, compositions, uses, and a device using a special peroxide compound, in which reinfection by microorganisms in the last washing phases - either through a bactericidal action or through a bacteriostatic (germicidal) action - does not occur, a high degree of reuse of the process water is possible, and yet a sufficient bleaching action is obtained.
  • the present invention comprises a process for wet cleaning textile in at least five phases comprising a soaking phase, at least one sudsing phase, a rinsing phase, a bleaching phase, and a neutralization phase, in which in a second sudsing phase or in the rinsing phase a peroxy acid having at least 6 carbon atoms or a compound converted in situ into such a peroxy acid is added.
  • the bleaching step is thus physically combined with a second sudsing phase or the rinsing phase.
  • the same washing result can be obtained using a washing line having a lower capacity, or the overcapacity of the washing line can be utilized for other purposes.
  • a peroxy acid having a somewhat longer hydrocarbon residue, or a compound converted into it during the washing process By using in the process according to the invention a peroxy acid having a somewhat longer hydrocarbon residue, or a compound converted into it during the washing process, a surprisingly better disinfection and a good bacteriostatic action is obtained because at least part of the peroxy acid adheres to the fibers of the textile so that peroxy acid remains present in the laundry after washing and thus the disinfecting action of that peroxy acid also remains present after the neutralization phase.
  • the peroxy acid used according to the invention also remains active during storage- of the moist laundry until the drying process so that then the spore-forming microorganisms do not multiply either.
  • the above-mentioned peroxy acids are readily biodegradable. Processes are further known for formulating the above peroxy acids to fully safe products. Safe products can be in the form of granules or aqueous suspensions. For use in wet cleaning processes preference is given to suspensions. Compositions of insoluble peroxycarboxylic acids containing alkyl groups and suspended in water are, as stated above, extensively described in the prior art. A feature of such suspensions is that they contain additives preventing the sagging or creaming of the peroxy compounds.
  • Known stabilizing agents are described in GB-A-153 504, EP-A-0 160 342, EP-A-0 176 124, EP-A-0 188 025, EP-A-0 201 958, EP-A-0 283 791, EP-A-0 283 792, EP-A-0 347 988, and EP-A-0 386 566.
  • compositions further comprise additives for ensuring or at least improving chemical stability.
  • additives for ensuring or at least improving chemical stability comprise the addition of specific sequestering agents and the limitation of the acidity to a pH in the range of 3 to 5.
  • the process according to the invention preferably makes use of a suspension free of surface active compounds.
  • This suspension can be dosed into the washing tube in the final phase of the washing process.
  • a suspension with which excellent results are obtained in the process according to the invention comprises 20-35%, preferably 25-30%, most preferably 27% DPDDA; 2-5%, preferably 3-4% sodium sulfate; about 0.2% xanthane gum; and about 0,2% hydroxyethyl cellulose in water having a pH adjusted to a value in the range of 3 to 4, preferably 3.7.
  • the percentage of active oxygen is about 3%.
  • the specific composition is readily pumpable and phase-stable.
  • the amount of peroxy acid required per kg of laundry and/or per liter of washing liquid is not directly critical and is substantially determined by the degree of pollution of the laundry, the amount of peroxy acid will mostly range between 10 and 50 mmol per kg of dry laundry, which corresponds to 2 to 10 mmol per liter of washing liquid.
  • This acid can be both an inorganic acid, e.g. phosphoric acid, and an organic acid. If preference is given to the use of an organic acid, in particular acetic or formic acid is used.
  • the acid is preferably added in such an amount that a pH of 7.5 to 5, preferably between 7 and 6, is obtained in the laundry, which for formic acid corresponds to, e.g. , 1 g per kg of dry laundry.
  • the washing process according to the invention is therefore carried out at a temperature between 25 and 75°C, in particular at a temperature between 45 and 65°C.
  • the processes according to the invention can be carried out within broad limits for the pH.
  • the neutralization phase the process is carried out with acid, hence the pH is lower then, also for the purpose of better activating the peroxy acids.
  • Fig. 4 shows a washing process according to the invention in which at different places process water is fed back into the washing process.
  • the process water to be fed back it is subjected to a purification step.
  • the lower washing temperature which can be obtained because of the better chemical disinfection of the laundry by the peroxy acids according to the invention enables a much more intensive reuse of the water.
  • the peroxy acids for use in the invention can be added in the washing process in many ways, e.g. in a solution with conventional solvents, as a granulate with the conventional fillers, as a suspension, or as a paste. They can also be added together with the washing agent in the (or the first or second) sudsing phase.
  • the peroxy acids according to the invention and the processes according to the invention can be combined with all conventional further treatments of the laundry. They can be used in processes with the conventional steps and with the conventional agents, particularly in the so-called industrial wet cleaning processes in which washing tubes or washing lines are used.
  • the industrial wet cleaning process is generally carried out with the following agents. Soap and/or detergents
  • soaps are still being used regularly, particularly in combination with synthetic detergents.
  • Soaps are in general sodium and/or potassium salts of fatty acids.
  • the sodium salts generally give hard soaps, whereas the potassium salts give the soft soaps.
  • the anionic washing agents include, inter alia, known alkylaryl sulfates, alkyl sulfonates, alkyl sulfates, sulfated alkylene oxide condensates, etc.
  • ⁇ on-ionic washing agents are, inter alia, alkyl polyglycol ethers, amine oxides, polyalkyl saccharides, etc.
  • Cationic compounds are in general quaternary ammonium compounds in which two substituents of the nitrogen atom are alkyl groups having 16 or more carbon atoms.
  • a frequently used additive to washing agents is, e.g., sodium carboxymethyl cellulose. Also, trinitriloacetic acid is often used. Besides, optical brightener, washing alkalis, soda, sodium metasilicate, sodium hydroxide, etc., are often used.
  • the composition of the washing agent can influence the pH, the bleaching action of the peroxy acid being optimal.
  • This optimum pH can be readily determined by a skilled man.
  • the constituents of washing agents having different functions, in particular the detergents, the basic additives, and the bleaching agents are often added in the washing process at different places in the correct concentration. In such a situation a suspension of a peroxy acid according to the invention is preferred because of the ability of being dosed.
  • compositions suitable for use in the process according to the invention are the following.
  • a first combination consists of a detergent mixture to be used in the soaking phase and the sudsing phase, comprising 0-60% fatty acid soap, 5-70% non-ionic detergent, 0-5% of a conventional isotropic aid, and water; a basic builder, comprising 0-60% soda, 0-80% sodium metasilicate, 0.1-2% sodium carboxymethyl cellulose, 0-1% optical brightener, 0-20% sodium triphosphate, and 0-2% ⁇ TA.
  • a second composition is formed by a complete powder to be used both in the soaking bath and in the sudsing phase, comprising at least 5% surfactant, 0-20% soda, 1-60% sodium metasilicate, 0-10% sodium hydroxide, 0.1-2% sodium carboxymethyl cellulose, 0-1% optical brightener, 0-40% sodium triphosphate, and 0-1% TA.
  • Fig. l gives an example of a washing process in five phases. 1 is the soaking phase, 2 is the sudsing phase, 3 is the rinsing phase, 4 is the bleaching phase, and 5 represents the neutralization phase.
  • Fig. 2 shows a washing tube suitable for carrying out the classical hypochlorite process in which the temperatures of the process water in the different phases can be expressed in °C.
  • the full arrows represent the water streams; the broken arrows represent the water streams to be fed back; and the numerals represent the amount of water to be discharged.
  • Fig. 3 shows a hydrogen peroxide process with bisulfite neutralization in which the temperatures of the process water in the different phases are expressed in °C; the full arrows represent water streams; the discontinuous arrows represent the water to be fed back; and the numerals at the arrows express the amount of water to be discharged in units of 1/kg of laundry.
  • Fig. 4 shows an embodiment of a washing tube and a washing process according to the invention in which the temperatures of the process water in the different phases are expressed in °C; the full arrows represent water streams; the broken arrows represent the water to be fed back; and the numerals represent the amount of water to be discharged.
  • a washing tube Charged into a washing tube according to the invention, as shown in Fig. 4, are 1200 kg of laundry (per hour), together with patches provided with standard dirt (KWIJOVE (quartz, iron oxide, and fat) , VEKOPROP (fats, carbohydrates, and proteins) , and SUNAK (blackcurrant juice) , obtainable from IR-TNO, The Netherlands; and EMPA 111 (pig's blood), obtainable from EMPA, Switzerland) .
  • the soaking phase comprises a treatment lasting 9 minutes with 200 ml of washing agent at an average temperature of 40°C and an average pH of 10.5.
  • the laundry is then subjected to a sudsing phase for 12 minutes.
  • the sudsing phase comprises 330 ml of washing agent and is carried out at an average temperature of 66°C and an average pH of 10.
  • the laundry is then subjected to a second sudsing phase, comprising no washing agent but DPDDA (1.3 g/kg of laundry) .
  • the laundry is then rinsed for 6 minutes and neutralized with 2.5 g/kg of laundry acetic acid.
  • the dosage of the acid was so selected that in the neutralization phase a pH in the range of 8 to 4, preferably of 7 to 5, was obtained. If the pH attains a value above 8, the laundry turns yellow; whereas a pH below 4 can lead to corrosion at the plants.
  • a pH in the range of 8 to 4 preferably of 7 to 5
  • the laundry turns yellow; whereas a pH below 4 can lead to corrosion at the plants.
  • 80% of the water is discharged, purified and fed back to the soaking phase.
  • In the neutralization phase 10% of the water is discharged, and 90% is fed back to the second sudsing phase and to the soaking phase. Of the water released during neutralization and pressing of the laundry, everything is fed back to the soaking phase.
  • test material After neutralization the test material is judged by the removal of the model dirt by measuring the (blue) light remission in a manner known to the skilled man.
  • the hygiene is tested by subjecting water and textile samples to conventional microbiological studies.
  • Charged into a washing tube according to the invention are 1200 kg of laundry (per hour) , together with patches with standard soils (VEKOPROP, KWIJOVE, SU ⁇ AK, and EMPA 111) .
  • the soaking phase comprises a treatment lasting 9 minutes with 60 ml of washing agent at an average temperature of 39°C and an average pH of 10.6.
  • the laundry is then subjected to a sudsing phase for 12 minutes.
  • the sudsing phase comprises 2.5 1 of washing agent and is carried out at an average temperature of 82°C and an average pH of 11.5.
  • the laundry is subjected to a bleaching phase, comprising hypochlorite (20 ml/kg of laundry) .
  • a bleaching phase comprising hypochlorite (20 ml/kg of laundry) .
  • the laundry is then rinsed for 6 minutes and neutralized with 2.5 g/kg of laundry bisulfite.
  • test material After neutralization the test material is judged by light remission. Hygiene is tested by taking bacteriological samples.
  • Table 3 shows the results of the bacteriological studies to which reference is made in Examples 1 and 2. More in particular, it has been determined how many spore-forming bacteria are present per ml of suds for reuse and per ml of liquid from the press.
  • the number of spore-forming bacteria is so much lower in the processed washing liquids that they are very suitable for reuse.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Detergent Compositions (AREA)

Abstract

Procédés de nettoyage de textiles à l'aide de processus de nettoyage par voie humide, effectués notamment dans des tubes de lavage. On a mis au point un procédé de nettoyage de textiles par nettoyage par voie humide, comportant au moins cinq phases, à savoir une phase d'imprégnation, au moins une phase de savonnage, une phase de rinçage, une phase de blanchiment et une phase de neutralisation, un peroxyacide ayant au moins 6 atomes de carbone, ou un composé transformé in situ en peroxyacide de ce type, étant ajouté pendant une seconde phase de savonnage ou pendant la phase de rinçage. On a également prévu l'utilisation comme agent désinfectant ou bactériostatique et/ou comme agent décolorant dans un tel processus, d'un peroxyacide ayant au moins 6 atomes de carbone, ou d'un composé produisant in situ un peroxyacide ayant au moins 6 atomes de carbone.
EP94926403A 1993-07-30 1994-07-29 Peroxyacides ou leurs precurseurs utilisables dans le nettoyage des textiles, et procedes de nettoyage de textiles a l'aide de ces peroxyacides ou de leurs precurseurs Withdrawn EP0711337A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
NL9301339A NL9301339A (nl) 1993-07-30 1993-07-30 Peroxyzuren of voorlopers daarvan voor de toepassing in het reinigen van textiel, alsmede werkwijzen en inrichtingen voor het reinigen van textiel met behulp van dergelijke peroxyzuren of voorlopers.
NL9301339 1993-07-30
PCT/NL1994/000177 WO1995004128A1 (fr) 1993-07-30 1994-07-29 Peroxyacides ou leurs precurseurs utilisables dans le nettoyage des textiles, et procedes de nettoyage de textiles a l'aide de ces peroxyacides ou de leurs precurseurs

Publications (1)

Publication Number Publication Date
EP0711337A1 true EP0711337A1 (fr) 1996-05-15

Family

ID=19862718

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94926403A Withdrawn EP0711337A1 (fr) 1993-07-30 1994-07-29 Peroxyacides ou leurs precurseurs utilisables dans le nettoyage des textiles, et procedes de nettoyage de textiles a l'aide de ces peroxyacides ou de leurs precurseurs

Country Status (4)

Country Link
EP (1) EP0711337A1 (fr)
AU (1) AU7625194A (fr)
NL (1) NL9301339A (fr)
WO (1) WO1995004128A1 (fr)

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EP2485400A1 (fr) 2009-01-26 2012-08-08 Fujitsu Semiconductor Limited Échantillonnage
US11180385B2 (en) 2012-10-05 2021-11-23 Ecolab USA, Inc. Stable percarboxylic acid compositions and uses thereof

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US8809392B2 (en) 2008-03-28 2014-08-19 Ecolab Usa Inc. Sulfoperoxycarboxylic acids, their preparation and methods of use as bleaching and antimicrobial agents
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US20140256811A1 (en) 2013-03-05 2014-09-11 Ecolab Usa Inc. Efficient stabilizer in controlling self accelerated decomposition temperature of peroxycarboxylic acid compositions with mineral acids
US8822719B1 (en) 2013-03-05 2014-09-02 Ecolab Usa Inc. Peroxycarboxylic acid compositions suitable for inline optical or conductivity monitoring
DE102013006200A1 (de) 2013-04-11 2014-10-16 Herbert Kannegiesser Gmbh Verfahren zum Nassbehandeln, vorzugsweise Waschen, von Wäschestücken
EP3766523A1 (fr) 2014-12-18 2021-01-20 Ecolab USA Inc. Génération d'acide peroxyformique par l'intermédiaire de formiate d'alcool polyhydrique
EP3232781A4 (fr) 2014-12-18 2018-08-22 Ecolab USA Inc. Procédés de formation d'acide peroxyformique et ses utilisations
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EP3904526B1 (fr) 2015-09-10 2024-07-10 Ecolab USA Inc. Produit chimique antimicrobien auto-indicateur
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
EP2485400A1 (fr) 2009-01-26 2012-08-08 Fujitsu Semiconductor Limited Échantillonnage
EP2485399A1 (fr) 2009-01-26 2012-08-08 Fujitsu Semiconductor Limited Échantillonnage
US11180385B2 (en) 2012-10-05 2021-11-23 Ecolab USA, Inc. Stable percarboxylic acid compositions and uses thereof

Also Published As

Publication number Publication date
NL9301339A (nl) 1995-02-16
AU7625194A (en) 1995-02-28
WO1995004128A1 (fr) 1995-02-09

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