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WO1997030098A1 - Procede d'agglomeration du liege - Google Patents

Procede d'agglomeration du liege Download PDF

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Publication number
WO1997030098A1
WO1997030098A1 PCT/EP1997/000355 EP9700355W WO9730098A1 WO 1997030098 A1 WO1997030098 A1 WO 1997030098A1 EP 9700355 W EP9700355 W EP 9700355W WO 9730098 A1 WO9730098 A1 WO 9730098A1
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WO
WIPO (PCT)
Prior art keywords
process according
composition
isocyanate
weight
cork
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.)
Ceased
Application number
PCT/EP1997/000355
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English (en)
Inventor
Stefan Emiel Jozef Ghislain Priemen
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.)
Imperial Chemical Industries Ltd
Original Assignee
Imperial Chemical Industries 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
Application filed by Imperial Chemical Industries Ltd filed Critical Imperial Chemical Industries Ltd
Priority to AU15954/97A priority Critical patent/AU1595497A/en
Publication of WO1997030098A1 publication Critical patent/WO1997030098A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/007—Cork
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes

Definitions

  • This invention relates to a process for binding cork and in particular a process for binding cork using isocyanate-containing prepolymers as binders.
  • organic polyisocyanates as binders for lignocellulosic material such as cork in the manufacture of sheets or moulded bodies such as cork panels or cork bottle stoppers is well known.
  • the organic polyisocyanate optionally in the form of a solution, dispersion or aqueous emulsion, is applied to the lignocellulosic material which is then subjected to heat and pressure.
  • polyisocyanates aliphatic, cycloaliphatic and, preferably, aromatic polyisocyanates are used as are their partial reaction products with isocyanate-reactive compounds such as polyols (so-called prepolymers) .
  • the present invention provides a process for binding cork comprising the steps of a) bringing said cork in contact with a polyisocyanate composition and b) subsequently allowing said cork to bind, wherein the polyisocyanate composition comprises an isocyanate-containing prepolymer composition having an NCO content of from 2 to 25 % by weight, preferably 2 to 15 %, most preferably 2 to 7 % by weight as obtainable by reacting an isocyanate-reactive polymer composition having an average nominal functionality of from 1.8 to 6, preferably 2 to 4, and an average equivalent weight of from 500 to 7000 with a stoichiometric excess of a diphenylmethane diisocyanate (MDI) composition.
  • MDI diphenylmethane diisocyanate
  • nominal functionality refers to the functionality, with respect to isocyanates, that an isocyanate-reactive polymer would be expected to have with regards to its monomeric components.
  • the average nominal functionality is the average functionality (number of active hydrogen atoms) of the initiator or initiators used in its preparation.
  • the diphenylmethane diisocyanate composition used to make the prepolymers can contain so-called polymeric MDI which is a mixture of diphenylmethane diisocyanates and higher functional oligomers thereof. Thus mixtures can be used containing pure MDI and so-called polymeric MDI.
  • the average isocyanate functionality of the MDi composition is preferably from 2 to 2.3 although higher functionality MDI compositions can be used as well.
  • the MDI composition contains at least 60 %, preferably 100 % by weight of difunctional MDI's: 2,4*-, 2,2*- and 4,4'-isomers of diphenylmethane diisocyanate and mixtures thereof.
  • the MDi composition preferably contains at least 60 % , preferably at least 85 % and more preferably at least 95 % on a weight basis of diisocyanate components of
  • Suitable isocyanates therefore include isomer mixtures containing not more than 40 %, preferably not more than
  • Unmodified forms of MDI can be used as well as modified forms that is to say MDI modified in known manner by the introduction of urethane, allophanate, urea, biuret, carbodiimide, uretonimine or isocyanurate residues.
  • MDI variants particularly include uretonirmne-modified MDI having NCO contents of at least 25 % by weight and polyether-based prepolymers having NCO contents of at least 20 % by weight.
  • Still further diphenylmethane diisocyanate compositions which may be used n preparing the prepolymer include mixtures of the above described MDI types and up to 20 % by weight of another polyisocyanate or mixture of polyisocyanates.
  • Other polyisocyanates which may be used in admixture with the MDI include aliphatic, cycloaliphatic and araliphatic polyisocyanates, especially dusocyanates, for example hexamethylene diisocyanate, isophorone diisocyanate, cyclohexane-1,4-d ⁇ socyanate, 4,4'-dicyclohexylmethane dusocyanates and m- and p-tetramethylxylene dusocyanates and, especially, aromatic polyisocyanates such as tolylene dusocyanates and phenylene dusocyanates.
  • the average nominal functionality of the isocyanate-reactive polymer is preferably 2 to 4, more preferably 2 to 3.
  • Preferred average equivalent weights lie in the range from 1000 to 5000.
  • Mixtures of two or more isocyanate-reactive polymers varying in functionality, equivalent weight and/or chemical constitution (end groups or backbone) may be used provided such mixtures conform to the average functionality and average equivalent weight criteria specified herein.
  • isocyanate-reactive polymers having functionalities and equivalent weights net within the specified ranges can be used.
  • isocyanate-reactive polymers known for use in the manufacture of rigid polyurethane foams having functionalities of 2 to 8 and equivalent weights of 10 to 750 can be used provided the total isocyanate- reactive composition conforms to the average functionality and average equivalent weight criteria specified herein.
  • Isocyanate-reactive groups which may be present m the isocyanate-reactive polymer include primary amine, secondary amine, thiol, carboxy, enamino and, especially, hydroxyl groups.
  • Particularly important isocyanate-reactive polymers include polymeric polyols.
  • Suitable polyols and methods for their preparation have been fully described in the prior art and, as examples of such polyols, there may be mentioned polyesters, polyesteramides, polythioethers, polycarbonates, polyacetals, polyolefms, polysiloxanes"and, especially, polyethers.
  • Polyether polyols which may be used include products obtained by the polymerisation of a cyclic oxide, for example ethylene oxide, propylene oxide, butylene oxide or tetrahydrofuran in the presence, where necessary, of polyfunctional initiators.
  • Suitable initiator compounds contain a plurality of active hydrogen atoms and include water and polyols, for example ethylene glycol, propylene glycol, diethylene glycol, cyclohexane dimethanol, resorcmol, bisphenol A, glycerol, tnmethylolpropane, 1,2,6- hexanet ⁇ ol or pentaerythritol. Mixtures of initiators and/or cyclic oxides may be used.
  • Especially useful polyether polyols include polyoxypropylene diols and triols and poly(oxyethylene-oxypropylene) diols and triols obtained by the simultaneous or sequential addition of ethylene and propylene oxides to di- or trifunctional initiators as fully described in the prior art.
  • Random copolymers having oxyethylene contents of 10 to 80 S, block copolymers having oxyethylene contents of from 2 to 30 ⁇ , preferably from 5 to 25 % and random/block copolymers having oxyethylene contents of up to 50 %, based on the total weight of oxyalkylene units may be mentioned. Mixtures of the said diols and triols can be particularly useful.
  • polyether polyols include polytetramethylene glycols obtained by the polymerisation of tetrahydrofuran. Particularly useful are also mixtures of polypropylene-polyethylene oxide polyols with up to 5 ⁇ of another polyol, for example a polyalkylene oxide, a polyester polyol, a polycarbonate polyol, a polyacetal polyol or a polytetramethylene glycol.
  • a particularly interesting category of polyol components consists of polyether polyols having an average oxyethylene content of from 10 to 25 * by weight of total oxyalkylene residues due to the presence therein of at least one polyoxyalkylene polyol containing oxyethylene (ethylene oxide) residues.
  • Preferred polyol components comprise at least one poly(oxyethylene-oxypropylene) polyol each having an oxyethylene content in the range from 10 to 25 % on a weight basis of total oxyalkylene residues.
  • polystyrene resin examples include poly(oxyethylene-oxypropylene) polyols, polyoxypropylene polyols and/or polyoxyethylene polyols, having oxyethylene contents outside the 10 to 25 % range provided the overall oxyethylene content of the component is within the specified range.
  • Such mixtures may optionally contain one or more poly(oxyethylene-oxypropylene) polyol having an oxyethylene content in the 10 to 25 % range.
  • mixtures of two or more polyols varying in functionality, equivalent weight and/or polymer backbone may be used provided such mixtures conform to the average functionality and average equivalent weight criteria specified herein.
  • Polyester polyols which may be used include hydroxyl-terminated reaction products of polyhydric alcohols such as ethylene glycol, propylene glycol, diethylene glycol, 1, -butanediol, neopentyl glycol, 1, 6-hexanediol, cyclohexane dimethanol, bis (hydroxylethyl) terephthalate, glycerol, trimethylolpropane, pentaerythritol or polyether polyols or mixtures of such polyhydric alcohols, and polycarboxylic acids, especially dicarboxylic acids or their ester-forming derivatives, for example succinic, glutaric and adipic acids or their dimethyl esters, sebacic acids, phthalic anhydride, tetrachlorophthalic anhydride or dimethyl terephthalate or mixtures thereof.
  • polyhydric alcohols such as ethylene glycol, propylene glycol, diethylene glycol, 1, -butaned
  • Polyesteramides may be obtained by the inclusion of aminoalcohols such as ethanolamine in polyesterification mixtures. Polyesters obtained by the polymerisation of lactones, for example caprolactone, in conjunction with a polyol, or of hydroxy carboxylic acids such as hydroxy caproic acid, may also be used.
  • Polythioether polyols which may be used include products obtained by condensing thioglycol either alone or with other glycols, alkylene oxides, dicarboxylic acids, formaldehyde, amino-alcohols or aminocarboxylic acids.
  • Polycarbonate polyols which may be used include products obtained by reacting diols such as 1, 3-propanediol, 1, -butanediol, 1,6-hexanediol, diethylene glycol or tetraethylene glycol with diaryl carbonates, for example diphenyl carbonate, or with phosgene.
  • diols such as 1, 3-propanediol, 1, -butanediol, 1,6-hexanediol, diethylene glycol or tetraethylene glycol
  • diaryl carbonates for example diphenyl carbonate, or with phosgene.
  • Polyacetal polyols which may be used include those prepared by reacting glycols such as diethylene glycol, triethylene glycol or hexanediol with formaldehyde. Suitable polyacetals may also be prepared by polymerising cyclic acetals.
  • Suitable polyolefin polyols include hydroxy-terminated butadiene homo- and copolymers and suitable polysiloxane polyols include polydimethylsiloxane diols and triols.
  • isocyanate-reactive polymers for preparing the prepolymers include polymeric polyamines, especially diamines and triamines, corresponding to the above described polymeric polyols.
  • Polyoxypropylene diamines and triamines and mixtures thereof are preferred.
  • polymers containing both amino and hydroxyl groups obtained by the partial amination of polyols.
  • isocyanate-reactive polymers which may be used in preparing the prepolymers include imino-functional polymers. Such polymers have been described in US-P-4794129 together with methods for their preparation and include polymers terminating in imine, oxazoline, imidazoline, N-alkyl imidazoline, oxazine, diazine, imino-ester, amidine, imidine, isourea and guanidine groups.
  • the preferred imino-functional polymers are imine- terminated polyethers such as may be obtained, for example by reacting a polyether polyamine, especially a polyoxypropylene diamine or triamine, with an aldehyde or ketone.
  • Enamine functional polymers may be prepared either from secondary amine terminated resins (i.e. polyethers) by reaction with ketones/aldehydes having one or more alpha hydrogens, or by reacting ketone/aldehyde terminated resins (bearing alpha hydrogens) with secondary amines, providing for removal of the water formed in the reactions.
  • Secondary amine terminated resins can be obtained, for example by catalytic hydrogenation of the imino-functional polymers described hereinabove.
  • Ketone/aldehyde terminated resins may be obtained, in general, by oxidation of the corresponding secondary or primary hydroxyl terminated resin.
  • More highly enamine functional polymers can be prepared by oxidising a primary hydroxy functional resin to the corresponding polycarboxylic acid, conversion of the said groups to orthoesters, end treatment of the latter, with an excess of a secondary amine.
  • Each orthoester must contain at least one alpha hydrogen atom.
  • the isocyanate-terminated prepolymer may be prepared by reacting the diphenylmethane diisocyanate composition with the isocyanate-reactive polymer under conditions that have been fully described in the prior art for the preparation of prepolymers.
  • an initial ratio of isocyanate to isocyanate-reactive groups would typically be within the range from 3:1 to 20:1.
  • Preferred prepolymers are made by reacting the starting materials at initial ratio of isocyanate to isocyanate-reactive groups in the range 3.5:1 to 15:1, especially 4:1 to 10:1, to give prepolymers having NCO contents of 4 to 12 S.
  • the viscosity of the prepolymer for use in the present process is preferably between 1500 and 8000 cP but can be higher as well.
  • the lower volatility of MDI relative to TDI is an advantage to the use of MDI prepolymers in the present process from the industrial hygiene point of view. In terms of resilience and flexibility similar properties as with TDI prepolymers are obtained.
  • the moulded cork bodies are prepared by bringing the cork into contact with the polyisocyanate composition like by means of mixing, spraying and/or spreading the composition with/onto the cork parts and by pressing the combination of the polyisocyanate composition and the cork parts, preferably by hot-pressing although curing at room temperature is possible as well.
  • Such binding processes are commonly known in the art.
  • Granulated cork material is fed into a mixer, e.g., a horizontal helicoidal mixer, mixing extruder or conventional mixing equipment for production of composites.
  • a well defined quantity of polyisocyanate adhesive is slowly poured over the granulates or fed into the extruder, while continuing mixing or blending, in order to obtain a homogeneous distribution of the binder and to obtain a uniform mixture.
  • Mixing time can range from a few seconds to 20 minutes. Some water or hydrophobic waxes may be added.
  • moulds are filled by extrusion or by pouring the treated cork material into them and cured under pressure. Temperature and moisture level determine the cure time.
  • Moisture level may vary between 2 and 20 i . Temperature may vary between 20 and 150°C.
  • the polyisocyanate composition for use in the present process may contain conventional additives such as release agents.
  • polyisocyanate compositions may be applied in such amounts to give a weight ratio of polyisocyanate/cork material in the range of 0.1:99.9 to
  • Density of the obtained cork bodies is usually in the range 250 to 750 kg/m 3 .
  • the cork bodies can be in the form of blocs which are cut into panels for use e.g. as floor tiles or in the form of stoppers for bottles.
  • MDI prepolymers were made from pure 4, '-MDI and various polyols at different NCO values.
  • the polyols used and the NCO value of the obtained prepolymers are given in Table 1.
  • Polyol 1 is a polyoxyalkylene polyol of molecular weight 6000 and average functionality 2.3, initiated with a triol; oxyethylene content is 15 % .
  • Polyol 2 is a polyoxyalkylene polyol of molecular weight 3740 and average functionality 1.8, initiated with a diol; oxyethylene content is 15 %.
  • Polyol 3 has a molecular weight of 2000 and average functionality 2; Arcol 1020 available from ARCO Chem Corp.
  • the MDI-prepolymers were mixed with cork at a loading of 25 % on cork weight basis.
  • An ANCHOR mixer was used to distribute the prepolymer on the cork. The prepolymer was added while the cork was stirred in a bucket.
  • Cork mats of 14 x 14 x 0.5 cm and density 450 kg/m 3 were made using a pressure of 100 bar, a temperature of 125°C and a press time of 3 minutes.
  • the polyol component was added to the polyisocyanate over a 30 min period gradually heating the reaction mixture up to 85 ⁇ C;
  • reaction mixture was heated and stirred for a further two hours to let reaction take place;
  • reaction mixture was cooled down to 60 C C and poured into a storage container.
  • the prepolymers were mixed with the cork granules on a 25 % weight ratio to the cork weight. Cork granules were stirred with an anchor mixer in a bucket while dripping in the isocyanate prepolymer.
  • cork mats were tested by means of a tensile test performed on a dumb ⁇ bell shaped sample (standard DIN 53571) . Three samples were tested from each mat. The results are presented in Table 3.
  • Polyol 4 being a polyoxyalkylene polyol of molecular weight 5250 and average functionality 2.4, initiated with glycerol;
  • Polyol 5 being a polyoxyalkylene polyol of molecular weight 2158 and average functionality 1.9, initiated with diethyleneglycol;
  • Polyol 6 being a polyoxyalkylene polyol of molecular weight 300 and average functionality 2.9, initiated with sorbitol.
  • the prepolymers were mixed with the cork granules on a 12 % weight ratio to the cork weight. Mixing was done by dripping the prepolymer into the granules under constant stirring.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

L'invention concerne un procédé d'agglomération du liège consistant: a) à mettre en contact le liège avec une composition de polyisocyanate et b) à permettre ultérieurement l'agglomération du liège. Cette composition de polyisocyanate comprend une composition prépolymère contenant de l'isocyanate dont la teneur en NCO est comprise entre 2 et 25 % en poids, cette composition pouvant être obtenue par la réaction d'une composition polymère, réagissant à l'isocyanate dont la fonctionnalité nominale moyenne est comprise entre 1, 8 et 6, et dont le poids équivalent moyen est compris entre 500 et 7000, avec un excédent stoéchiométrique d'une composition de diphénylméthane diisocyanate.
PCT/EP1997/000355 1996-02-19 1997-01-27 Procede d'agglomeration du liege Ceased WO1997030098A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU15954/97A AU1595497A (en) 1996-02-19 1997-01-27 Process for binding cork

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP96102449.4 1996-02-19
EP96102449 1996-02-19

Publications (1)

Publication Number Publication Date
WO1997030098A1 true WO1997030098A1 (fr) 1997-08-21

Family

ID=8222488

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1997/000355 Ceased WO1997030098A1 (fr) 1996-02-19 1997-01-27 Procede d'agglomeration du liege

Country Status (6)

Country Link
AU (1) AU1595497A (fr)
ID (1) ID15962A (fr)
MA (1) MA24086A1 (fr)
TN (1) TNSN97038A1 (fr)
WO (1) WO1997030098A1 (fr)
ZA (1) ZA971288B (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2014723A1 (fr) 2007-07-11 2009-01-14 Basf Se Procédé de fabrication de corps moulés en liège
WO2011095713A2 (fr) 2010-02-08 2011-08-11 Jacques Granger Traitement de bouchons en liege naturel et bouchons obtenus par ledit traitement
DE102015210569A1 (de) * 2015-06-09 2016-12-15 Georg-August-Universität Göttingen Stiftung Öffentlichen Rechts Erhöhung der Reaktivität von Isocyanatklebstoffen durch Amin-/Ammoniumverbindungen

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1620777A1 (de) * 1965-09-29 1970-09-03 Cushioned Products Corp Verfahren zur Herstellung von Kork- und gegebenenfalls Schaumstoffteilchen enthaltenden Massen
DE2711958A1 (de) * 1977-03-18 1978-09-21 Bayer Ag Verfahren zur bindung oder impraegnierung lignocellulosehaltiger rohstoffe
EP0005473A1 (fr) * 1978-05-12 1979-11-28 Bayer Ag Procédé de fabrication de matières en couche et liant approprié pour l'exécution du procédé
EP0392788A2 (fr) * 1989-04-14 1990-10-17 Imperial Chemical Industries Plc Composition d'isocyanate et procédé de préparation de mousses flexibles à partir de celle-ci

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1620777A1 (de) * 1965-09-29 1970-09-03 Cushioned Products Corp Verfahren zur Herstellung von Kork- und gegebenenfalls Schaumstoffteilchen enthaltenden Massen
DE2711958A1 (de) * 1977-03-18 1978-09-21 Bayer Ag Verfahren zur bindung oder impraegnierung lignocellulosehaltiger rohstoffe
EP0005473A1 (fr) * 1978-05-12 1979-11-28 Bayer Ag Procédé de fabrication de matières en couche et liant approprié pour l'exécution du procédé
EP0392788A2 (fr) * 1989-04-14 1990-10-17 Imperial Chemical Industries Plc Composition d'isocyanate et procédé de préparation de mousses flexibles à partir de celle-ci

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2014723A1 (fr) 2007-07-11 2009-01-14 Basf Se Procédé de fabrication de corps moulés en liège
WO2011095713A2 (fr) 2010-02-08 2011-08-11 Jacques Granger Traitement de bouchons en liege naturel et bouchons obtenus par ledit traitement
DE102015210569A1 (de) * 2015-06-09 2016-12-15 Georg-August-Universität Göttingen Stiftung Öffentlichen Rechts Erhöhung der Reaktivität von Isocyanatklebstoffen durch Amin-/Ammoniumverbindungen

Also Published As

Publication number Publication date
ZA971288B (en) 1997-08-19
TNSN97038A1 (fr) 1999-12-31
ID15962A (id) 1997-08-21
AU1595497A (en) 1997-09-02
MA24086A1 (fr) 1997-10-01

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