EP0112744B1 - Procédé de neutralisation accélerée de substrats textiles cellulosiques et appareils de mise en oeuvre - Google Patents

Procédé de neutralisation accélerée de substrats textiles cellulosiques et appareils de mise en oeuvre Download PDF

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Publication number
EP0112744B1
EP0112744B1 EP83402269A EP83402269A EP0112744B1 EP 0112744 B1 EP0112744 B1 EP 0112744B1 EP 83402269 A EP83402269 A EP 83402269A EP 83402269 A EP83402269 A EP 83402269A EP 0112744 B1 EP0112744 B1 EP 0112744B1
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EP
European Patent Office
Prior art keywords
neutralization
carbon dioxide
treatment
substrate
neutralizing
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
Application number
EP83402269A
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German (de)
English (en)
French (fr)
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EP0112744A3 (en
EP0112744A2 (fr
Inventor
Jean-Pierre Zumbrunn
Jean Levielle
André Thomas
Françoise Grangette
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.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
TEINTURERIE DE CHAMPAGNE
Original Assignee
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
TEINTURERIE DE CHAMPAGNE
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Application filed by LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude, TEINTURERIE DE CHAMPAGNE filed Critical LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority to AT83402269T priority Critical patent/ATE21947T1/de
Publication of EP0112744A2 publication Critical patent/EP0112744A2/fr
Publication of EP0112744A3 publication Critical patent/EP0112744A3/fr
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B19/00—Treatment of textile materials by liquids, gases or vapours, not provided for in groups D06B1/00 - D06B17/00
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • D06M11/71—Salts of phosphoric acids

Definitions

  • the present invention relates to an accelerated neutralization process for cellulosic textile substrates and to processing apparatuses.
  • the textile industry and more particularly that of the development of particular qualities of cotton in yarn, woven, knitted, pure or in mixture uses techniques known as mercerization or caustification. These operations are carried out by bringing the cellulosic material into contact with an aqueous solution of caustic soda.
  • German patent 120,344 describes a mercerization method during which a treatment with carbon dioxide takes place in order to eliminate the shrinking effect of the sodium hydroxide solution.
  • the material having acquired the particular qualities sought leaves the mercerizing or causticizing machine, impregnated with sodium hydroxide solution. Pressing roller pressing makes it possible to limit the amount of soda lye entrained. Rinses are then carried out to remove the residual alkali.
  • cellulose has a great chemical affinity for soda, and the divided nature of the fibers is favorable for liquid retention by capillarity.
  • alkali-cellulose C 12 H 20 0 10 .2NaOH.
  • One of the conventional, discontinuous processes for removing alkali consists in practicing a succession of rinses requiring the use of repetitive loads of cold, hot, acidulated water on the same machine, for a given load of textile.
  • Another usual, continuous process consists in using a series of rinsing machines, in series, which can be tanks on casters; the textile scrolling continuously.
  • the total duration of the operations, including the idle times, is around two hours, or more if the hot rinse water is not preheated.
  • the continuous variant uses the same baths, in a succession of machines or enclosures.
  • the abundance of cold, hot or acidulated water volumes is essential to avoid any trace of residual alkali, detrimental to the quality and which can even disturb other subsequent operations, dyeing for example.
  • the neutralizing medium is at a temperature between 70 and 90 ° C.
  • Carbon dioxide vis-à-vis alkaline cellulosic textile substrates behaves like an active gas reacting on the one hand on caustic soda NaOH, and on the other hand on the chemical bond known as alkali-cellulose.
  • the direct reaction of carbon dioxide with free caustic soda and alkali-cellulose has the advantageous consequence of immediate in-situ neutralization, with formation in both cases of sodium hydrogen carbonate, known as sodium bicarbonate, practically neutral and harmless to the environment.
  • Another advantage of the present invention lies in the fact that the sodium bicarbonate, neutral salt does not disturb a possible subsequent operation of treatment of the caustified or mercerized textile, for example, bleaching or dyeing. Consequently, it is not always essential to rinse the neutralized textile load abundantly before said operation, which represents a saving of time and a saving of water.
  • the effluents leaving neutralization and its possible rinses are, by definition neutral or at a pH close to 8, at most 8.3, a value compatible with the standards for discharging waste water. Thus, they can be rejected directly, without further processing.
  • an accidental discharge of water loaded with sodium hydroxide which can therefore be at a pH of 10 to 14, well above the discharge tolerances, is not possible, which has a predominantly favorable impact on the risks. accidental pollution.
  • the reactions of alkali cellulose and caustic soda with carbonic acid H 2 CO 3 are practically instantaneous.
  • the neutralization time therefore only depends on the temperature, the speed of injection of carbon dioxide into the neutralization enclosure and of course, the capacity of the neutralization machine, to ensure rapid contact between the reagent and the products to be neutralized.
  • the contact between the substrate impregnated with free alkali hydroxide or fixed on cellulose and the neutralizing fluid containing carbon dioxide can be carried out in the gas phase, in the aqueous phase or in the combined gas and aqueous phases, the order of the phases being dependent of the type of continuous or discontinuous process.
  • the neutralizing fluid is introduced as a function of demand in relation to the quantity of alkali to be neutralized.
  • Carbon dioxide can be brought into contact with the cellulose substrate, impregnated with alkali hydroxide, in the gaseous state, which corresponds to the creation of a neutralizing atmosphere.
  • the water of said solutions can be brought to a temperature of 30 to 90 ° C, preferably 70 to 80 ° C, which significantly improves the kinetics of the reaction, compared to the use of cold water.
  • the technique of spraying an emulsion has the advantage of allowing the textile spun, therefore crushed by the pressure rollers of the mercerizing or causticizing machine, to regain volume by swelling under the action of the water emulsion - C0 2 - C0 3 H 2 from where supply to the heart, neutralizing solution and activation of the process.
  • the process of accelerated neutralization of cellulosic textile substrates with carbon dioxide is applicable in the treatment of textiles by the aqueous route in the continuous and discontinuous processes, in contact apparatus.
  • the in-situ neutralization technique consists of spraying on the textile material in constant movement, a gaseous stream of carbon dioxide or an aqueous emulsion water-C0 2 -C0 3 H 2 as previously described, with distribution at one or more points depending on the width of the textile sheet.
  • the gas or emulsion supply pressure is adjusted so that the neutralizing jet passes through the material and already performs a pre-neutralization to the core.
  • Neutralization being implemented in a closed enclosure, it remains permanently filled with carbon dioxide, which makes it possible to obtain contact with the textile material, conducive to possible additional neutralization with carbon dioxide gas.
  • the consumption of carbon dioxide by the alkali permeating the fibers can imply a depression inside the treatment enclosure, also a regulation of the gas pressure ensures the supply of carbon dioxide gas, with a view to neutralization complementary.
  • the regulation is independent of the textile impregnation rate and the alkali concentration, it only reacts to the demand for neutralizing gas, itself dependent on the presence of caustic soda and alkali-cellulose in the material. treatment.
  • This regulation mode gives great safety in use and allows a saving of reagent because, in case of stopping the introduction of alkaline textile or in case of passage of a non-alkaline product, the injection of fluid neutralizer will be automatically stopped as soon as the set pressure is reached.
  • the very short contact time between the textile material and the neutralizing reagent is compatible with the running speeds of the material.
  • aqueous phase It has been found advantageous to follow the previous neutralization phase, called the gaseous phase, with an aqueous phase.
  • the treatment in aqueous phase is carried out by impregnating the textile with water saturated with carbon dioxide. This impregnation with water containing carbonic acid H 2 CO 3 makes it possible to remove, if necessary, the last traces of the alkalinity of the textile while ensuring pre-rinsing.
  • the introduction of carbon dioxide into the water is controlled and adjusted so as to introduce carbon dioxide as soon as the pH of the aqueous impregnation solution returns to alkaline values.
  • This introduction is supplemented by a supply of fresh water and a purge, the flow rates of which are calculated so as to avoid the accumulation of sodium hydrogen carbonate.
  • the supply of fresh water is ensured by this injection, and it is therefore not necessary to renew the water of the base serving as a pre-rinse. Excess neutral water is removed continuously in a conventional manner.
  • a final rinse in water is carried out for the textile, considered as finished material. This rinsing can be brief if the textile undergoes a complementary bleaching or dyeing treatment because it is only impregnated with sodium hydrogen carbonate.
  • the characteristics of direct and accelerated neutralization are applicable in batch processes, and usable in contact apparatus.
  • the neutralization treatment is carried out by charge; the general principles of processing being identical to those set out for the continuous system.
  • a so-called gas phase neutralization treatment is carried out with the creation of an atmosphere of carbon dioxide.
  • this first treatment is completed by neutralization in the aqueous phase by impregnation in a saturated aqueous solution of carbon dioxide, or an emulsion ea U -C0 2 -CO 3 H 2 .
  • the treatment is preferably carried out in an enclosure filled with a carbon dioxide anhydride, preferably provided with a tank bottom containing dissolved carbon dioxide in which the textile is bubbled.
  • the textile strip the ends of which are connected to form a loop, circulates in the enclosure for neutralization, then rinsing.
  • the devices making it possible to implement the accelerated neutralization process for cellulosic substrates can be of a conventional type, to which are added a gas pressure detector, connected to a gas pressure regulator, in the sealed treatment enclosure in relation to a neutralizing fluid flow meter from a storage facility and means for distributing and injecting the neutralizing fluid.
  • the point of injection of the neutralizing fluid is located at the bottom of the treatment enclosure and the point of insertion of the detector in the upper half of said enclosure.
  • This equipment of the discontinuous dyeing machine type consists of a sealed sealed enclosure (1) provided with a turnstile (2), with a door or with an airlock system (3) for the introduction and removal of the textile.
  • This dyeing machine is equipped with a device specific to neutralization with carbon dioxide which comprises a gas pressure regulator (4) which controls the arrival of the neutralizing fluid, the detector member of the regulator (5) regulates a pressure gas in the enclosure (1) by controlling the distribution of carbon dioxide from a storage (6), via the flow meter (7) and the distribution piping (8) and the point of injection (9) at the bottom of the treatment enclosure.
  • the gas distribution via (7) and (4) is provided with a bypass (10) by which the air is purged, if necessary, while saturating the base of the vessel (11) by water, introduced by the valve (12), (used for filling or rinsing).
  • the valve (1) calibrated a few millibars above the calibration of the pressure regulator (4) allows the product to be evacuated from the purge and serves as an anti-pressure safety device.
  • the turnstile (2) is then started and circulates the sheet of fabric (14) both in the upper part of the enclosure (1) filled with carbon dioxide and in the foot the tank (11) water saturated with carbon dioxide.
  • the reaction for neutralizing sodium hydroxide in sodium hydrogen carbonate is instantaneous and its duration depends only on the capacity for introduction of carbon dioxide controlled by the pressure regulator (4); the consumption of carbon dioxide depends only on the alkaline demand provided by the fabric.
  • the indication of end of reaction is obtained by observation of the flow meter (7) which indicates the stopping of the circulation of carbon dioxide in the distribution circuit (8).
  • the water at the bottom of the tank, loaded with sodium bicarbonate, can be removed without further treatment by commissioning the purge valve (15).
  • a load of cotton fabric is introduced, leaving a causticizing machine, impregnated with causticizing liquor, the content of which, corresponding to caustic soda and alkali-cellulose, cumulative amount is 25 kg, expressed as NaOH.
  • the enclosure is optionally purged of its air while saturating the base with water, the valve being tared once and for all a few millibars above the setting of the gaseous pressure regulator of the enclosure.
  • the turnstile is started up so as to circulate the sheet of fabric both in the enclosure filled with C0 2 gas and in the bottom of the tank saturated with C0 2 .
  • the indication of end of reaction being given by the stopping of the passage of the gas flow visualized by the flow meter, a new water charge of 1,000 liters is optionally introduced for rinsing the 100 kg of neutralized tissue.
  • the bottom of the tank is heated to 70-80 ° C, for 10 minutes in the particular case of this example.
  • the time required for neutralization and rinsing is maximum 20 minutes.
  • a consumption of C0 2 of 29 kg is observed, ie a utilization yield of 95%.
  • the additional 5% of C0 2 corresponds to the inevitable losses due to leaks in the system.
  • Figure 2 of the accompanying drawing shows by way of example a continuous textile machine which includes the neutralization and rinsing installations.
  • This apparatus for vertical unwinding of textile consists of a sealed sealed enclosure comprising a vertical section in which the neutralizing treatment of the textile material in the gas phase is carried out, extended by a curved section in which the treatment in the aqueous phase is carried out , supplemented by the rinsing section proper and the vertical section for raising the treated fabric.
  • This assembly is as follows, taking the example of a sheet fabric leaving a causticizing machine, after expressing the excess sodium liquor by pressure rollers.
  • the upper part of the first vertical section (1) is provided with sealing means (2) such as flexible lips, the material to be treated (3) is introduced into the enclosure by a system of distributing rollers (13), the rotation speed adjusts the speed of the fabric.
  • This first part of this vertical section (1) of the downward unwinding of the cellulosic substrate is provided with at least one series of means (14) for projecting the neutralizing fluid, arranged perpendicularly to the direction of unwinding of the textile and to the two faces thereof. ci, upstream or downstream of the distributor rollers (13).
  • These spraying means (14) are of a conventional type, constituted for example by a series of nozzles or perforated tubes, placed opposite each side of the textile and staggered with respect to each other, so as to project an emulsion of carbon dioxide and water on the tissue with sufficient upstream pressure for the jets to pass through the tissue, without adversely affecting their effect, and allowing neutralization at the core.
  • the pressure of the neutralizing fluid is adjusted according to the thickness of the fabric.
  • FIG. III shows a representation of a ramp (14) of perforated tubes arranged on either side of the fabric, supplied with emulsion by a conventional mixer-emulsifier system (23) to which the C0 2 pipe (15) and the hot water pipe (16) (representation by a ramp).
  • a conventional mixer-emulsifier system (23) to which the C0 2 pipe (15) and the hot water pipe (16) (representation by a ramp).
  • the temperature of around 70 ° C for the water is favorable.
  • the fabric sheet After neutralization treatment by spraying-spraying at the nozzles (14), the fabric sheet approaches the middle and lower part (17) of the first vertical section, the atmosphere of which is formed by the projected excess carbon dioxide.
  • the length of this second section is determined so as to obtain a contact time of 15 to 30 seconds. Additional neutralization can be ensured if necessary, by introduction of gaseous carbon dioxide in (15) pilot by a regulator of the type described (4) with another detector (5).
  • the section of the enclosure (1) is delimited, at its upper part by the entry or sealing airlock (2) and at its lower part by the water level (11), the latter being contained in the curved part (12) of the installation, water level known as the base of the tank.
  • C0 2 is automatically regulated using a pressure regulator (4) identical to that described in figure (1), the detector (5) of which is placed in the vertical part charged with gas, for example at the level indicated on Figure II.
  • the pressure sensing member (5) controls the distribution of carbon dioxide via the flow meter (7) and the distribution pipes (10) and (8), the latter ending in (10), from the storage of C0 2 (6).
  • Neutralization safety the optional use of which depends on the degree of alkalinity of the fabric, is ensured by an additional injection of carbon dioxide in (9) inside the curved lower section (12) of the treatment, in the base (11).
  • This additional injection of carbon dioxide is controlled by a standard pH regulation of the base (11); this probe (18) being placed for example at the point indicated in FIG. II.
  • This so-called security system can absorb an exceptional point of alkalinity.
  • the fabric after neutralization treatment leaves the curved section (12) by an optional airlock (19), having the function of additional safety, although the carbon dioxide by the rollers (20), is drawn towards the rinsing section (21) then guided by the rollers (22), the rotational speed of which, coupled with that of the rollers (20) and (13), controls the movement of the fabric.
  • the liquid levels are adjusted by conventional devices such as overflows (not shown), and the water flow rates are adjusted according to the criteria for elimination of the hydrogen carbonate, to avoid its accumulation.
  • a system of safety valve (24) and bypass (25) of the pressure regulator is arranged on the treatment enclosure to allow it to be purged of air.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
EP83402269A 1982-11-29 1983-11-24 Procédé de neutralisation accélerée de substrats textiles cellulosiques et appareils de mise en oeuvre Expired EP0112744B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT83402269T ATE21947T1 (de) 1982-11-29 1983-11-24 Verfahren zur beschleunigten neutralisierung von zellulosehaltigen, textilen substraten und vorrichtung zu dessen durchfuehrung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8219963A FR2536769B1 (fr) 1982-11-29 1982-11-29 Procede de neutralisation acceleree de substrats textiles cellulosiques et appareils de mise en oeuvre
FR8219963 1982-11-29

Publications (3)

Publication Number Publication Date
EP0112744A2 EP0112744A2 (fr) 1984-07-04
EP0112744A3 EP0112744A3 (en) 1984-10-24
EP0112744B1 true EP0112744B1 (fr) 1986-09-03

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EP83402269A Expired EP0112744B1 (fr) 1982-11-29 1983-11-24 Procédé de neutralisation accélerée de substrats textiles cellulosiques et appareils de mise en oeuvre

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US (1) US4536907A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
EP (1) EP0112744B1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
JP (1) JPS59112066A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
AT (1) ATE21947T1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
AU (1) AU555376B2 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
CA (1) CA1195052A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
DE (1) DE3365907D1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
ES (1) ES527590A0 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
FR (1) FR2536769B1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
ZA (1) ZA838751B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)

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US5295998A (en) * 1993-02-02 1994-03-22 Liquid Carbonic Industries Corporation Adjusting pH in dyeing processes using CO2
DE19704797B4 (de) * 1997-02-08 2005-11-17 Krüger, Rudolf, Dr. Verfahren zum kontinuierlichen Färben von cellulosehaltigem Garn mit Indigo in einem einzigen Zug unter Steuerung des ph-Wertes
AU2729401A (en) * 1999-12-28 2001-07-09 Kimberly-Clark Worldwide, Inc. Fibrous materials
ITMI20021220A1 (it) * 2002-06-05 2003-12-05 Savio Macchine Tessili Spa Procedimento e dispositivo per il mercerizzo in continuo dei filati tessili
DE10349375B4 (de) * 2003-10-21 2008-04-10 Then Maschinen (B.V.I.) Ltd., Road Town Verfahren und Vorrichtung zum Spülen von strangförmigen Textilgut
US7235110B2 (en) * 2004-02-18 2007-06-26 Melvin Alpert Method for dyeing fabric materials with indigo, other vat dyes, and sulfur dyes
US6997962B2 (en) * 2004-02-18 2006-02-14 Melvin Alpert Method for dyeing cotton with indigo
EP1995374A2 (en) 2007-05-09 2008-11-26 Denimart S.A.de C.V. Textile products dyed by means of cationic dyes, and process for the manufacture thereof.
ES2428765B1 (es) 2013-10-04 2014-03-27 Tejidos Royo S.L. Tejido Denim con características ignífugas y proceso de tintura de la urdimbre con colorante azul índigo
KR102200028B1 (ko) * 2017-11-07 2021-01-08 주식회사 엘지화학 기체 분리막의 제조방법 및 이에 의하여 제조된 기체 분리막
WO2023155129A1 (en) * 2022-02-18 2023-08-24 Linde Gmbh Ph control in a dyeing process using co2
CN114775201B (zh) * 2022-04-15 2024-01-30 广东溢达纺织有限公司 一种利用二氧化碳气体调节织物pH的系统和方法

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Publication number Publication date
AU2169883A (en) 1984-06-07
JPH0377303B2 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1991-12-10
ES8406600A1 (es) 1984-08-01
FR2536769B1 (fr) 1985-09-27
AU555376B2 (en) 1986-09-18
EP0112744A3 (en) 1984-10-24
ES527590A0 (es) 1984-08-01
DE3365907D1 (en) 1986-10-09
FR2536769A1 (fr) 1984-06-01
JPS59112066A (ja) 1984-06-28
US4536907A (en) 1985-08-27
CA1195052A (fr) 1985-10-15
ZA838751B (en) 1984-07-25
EP0112744A2 (fr) 1984-07-04
ATE21947T1 (de) 1986-09-15

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